CN117488104A - Method for preparing high-vanadium slag by treating vanadium-containing slurry by fluidized bed - Google Patents
Method for preparing high-vanadium slag by treating vanadium-containing slurry by fluidized bed Download PDFInfo
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- CN117488104A CN117488104A CN202311446096.XA CN202311446096A CN117488104A CN 117488104 A CN117488104 A CN 117488104A CN 202311446096 A CN202311446096 A CN 202311446096A CN 117488104 A CN117488104 A CN 117488104A
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- fluidized bed
- titanium tetrachloride
- vanadium
- vanadium slag
- slurry
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 120
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 239000002002 slurry Substances 0.000 title claims abstract description 91
- 239000002893 slag Substances 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 87
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 83
- 238000002386 leaching Methods 0.000 claims abstract description 60
- 239000000446 fuel Substances 0.000 claims abstract description 49
- 238000007670 refining Methods 0.000 claims abstract description 29
- 239000000428 dust Substances 0.000 claims abstract description 25
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003546 flue gas Substances 0.000 claims abstract description 9
- 238000005507 spraying Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000003860 storage Methods 0.000 claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 claims abstract 3
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 239000007789 gas Substances 0.000 claims description 24
- 239000007790 solid phase Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 15
- 238000005243 fluidization Methods 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 239000004449 solid propellant Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000002006 petroleum coke Substances 0.000 claims description 7
- 239000006004 Quartz sand Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 239000011324 bead Substances 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 239000011335 coal coke Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 description 18
- 238000007599 discharging Methods 0.000 description 6
- 238000005660 chlorination reaction Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005262 decarbonization Methods 0.000 description 2
- 238000006298 dechlorination reaction Methods 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910021550 Vanadium Chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- 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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention relates to the technical field of high vanadium slag, and discloses a method for preparing high vanadium slag by treating vanadium-containing slurry by a fluidized bed, which comprises the steps of starting a circulating pump of a leaching system, spraying titanium tetrachloride into a leaching tower, and establishing a leaching system circulation; adding the fluidized material and fuel into a fluidized bed reactor through a metering screw, introducing air to react, and establishing a material layer; after the temperature in the bed reaches the required temperature, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, and the temperature of the fluidized bed and the temperature of flue gas are regulated by flow; cyclone dust collection system: alternately starting a cyclone blanking rotary valve 1 and a rotary valve 2, and collecting high vanadium slag; after the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby; and after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
Description
Technical Field
The invention relates to the technical field of high vanadium slag, in particular to a method for preparing high vanadium slag by treating vanadium-containing slurry by a fluidized bed.
Background
Titanium tetrachloride is the main raw material of industrial products such as titanium dioxide by a chlorination method and titanium sponge, and the main production methods at home and abroad comprise two methods of boiling chlorination and fused salt chlorination, the titanium tetrachloride produced by the two methods is purified by refining, vanadium-containing slurry produced in the process is treated by a heating evaporation furnace or a direct chlorination furnace, wherein the direct chlorination furnace can lead vanadium element in the slurry to enter waste residues along with slag and cannot be reused, the heating evaporation furnace is mainly used for evaporation treatment by intermittent operation and resistance heating, and the treated vanadium slag still needs secondary treatment of dechlorination and decarbonization, so that the treatment efficiency is low and the treatment cost is high. According to the invention, the vanadium-containing slurry is treated in a fluidized bed reactor mode, so that the treatment speed of the slurry is greatly improved, and vanadium slag generated after the reaction can be used as a raw material for producing vanadium products without secondary dechlorination and decarbonization treatment.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a method for preparing high-vanadium slag by treating vanadium-containing slurry by a fluidized bed, which improves the vanadium grade in slag and produces byproduct high-vanadium slag with high added value.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for preparing high vanadium slag by treating vanadium-containing slurry by a fluidized bed, which comprises the following steps:
(1) Starting a circulating pump of the leaching system, spraying titanium tetrachloride into the leaching tower, and establishing the circulation of the leaching system;
(2) Feeding system: adding the fluidized material and fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 10-18h, and establishing a material layer;
(3) After the temperature in the bed reaches 400-500 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, the temperature of the fluidized bed is controlled at 500-700 ℃ through flow regulation, and the temperature of flue gas is controlled at 200-300 ℃;
(4) Cyclone dust collection system: alternately starting a cyclone blanking rotary valve 1 and a rotary valve 2, and collecting high vanadium slag;
(5) After the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby;
(6) And after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
Preferably, the leaching system in the step (1) is used for collecting the gaseous titanium tetrachloride generated by the fluidized bed, wherein the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid phase matters, the solid phase matters are returned to the fluidized bed again through a mud return pipeline, the solid phase matters of the titanium tetrachloride collected by the leaching tower 2 are controlled to be 0.01-0.1g, the solid phase matters can be returned to the refining system again for purification, the heat exchanger is used for cooling the titanium tetrachloride, and the leached tail gas enters the tail gas system for washing and is discharged after reaching standards.
Preferably, the feeding system in (2) consists of a fluidization bin, a fuel bin, a metering screw and a mixing feeder, and is used for conveying the fluidization material and the fuel into the fluidized bed reactor.
Preferably, the fluidized material in the step (2) is fluidized material, quartz sand or zirconium bead inert material can be selected, and the inert material does not participate in the reaction and is used for establishing and accumulating a fluidized bed; the material of the fuel bin is fuel, and can be coal or petroleum coke solid fuel for the heat supply of the fluidized bed reactor.
Preferably, the fluidized bed reactor in (3) is composed of a fluidized bed reactor body, an air pipeline and a slurry adjusting pipeline, wherein the air pipeline is used for providing gas required by fluidized bed fluidization and oxygen required by reaction, the slurry adjusting pipeline is composed of a refining slurry pipeline and a circulating slurry pipeline, and the refining slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed to be matched with fuel feeding.
Preferably, the cyclone dust collection system in the step (4) consists of a cyclone dust collector, a rotary blanking valve and a high vanadium slag tank, and is used for separating substances generated after the reaction, the separated solid phase high vanadium slag enters the slag tank for collection, and the separated gas-phase titanium tetrachloride enters the leaching system for washing for 20-40min.
(III) beneficial technical effects
According to the invention, the vanadium-containing slurry is treated by the fluidized bed, so that titanium tetrachloride in the titanium tetrachloride slurry and vanadium-containing slag are rapidly separated, and vanadium chloride is reacted to generate vanadium pentoxide, so that the vanadium grade in the slag is improved, and the byproduct high-vanadium slag with high added value is produced.
Drawings
FIG. 1 is a schematic diagram of a fluidized bed treatment of vanadium-containing slurry to produce high vanadium slag.
Detailed Description
Example 1
(1) Starting a circulating pump of a leaching system, spraying titanium tetrachloride into a leaching tower, establishing a leaching system circulation, wherein the leaching system is used for collecting the gaseous titanium tetrachloride generated by a fluidized bed, the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid matters and returns to the fluidized bed again through a mud return pipeline, the titanium tetrachloride solid matters collected by the leaching tower 2 are controlled to be 0.01g, the titanium tetrachloride solid matters can return to a refining system again for purification, a heat exchanger is used for cooling the titanium tetrachloride, and the leached tail gas enters a tail gas system for washing and is discharged after reaching standards;
(2) Feeding system: adding fluidized materials and fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 10 hours, establishing a material layer, wherein a feeding system consists of a fluidized material bin, a fuel material bin, a metering screw and a mixed feeder and is used for conveying the fluidized materials and the fuel into the fluidized bed reactor, wherein the fluidized material bin is made of fluidized materials, quartz sand inert materials can be selected, and the inert materials do not participate in the reaction and are used for establishing and heat accumulating of the fluidized bed layer; the material of the fuel bin is fuel, and coal coke solid fuel can be selected for supplying heat to the fluidized bed reactor;
(3) After the temperature in the bed reaches 400 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, wherein the fluidized bed reactor consists of a fluidized bed reactor body, an air pipeline and a slurry adjusting pipeline, the air pipeline is used for providing gas required by fluidization of the fluidized bed and oxygen required by reaction, the slurry adjusting pipeline consists of a refined slurry pipeline and a circulating slurry pipeline, the refined slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed, the vanadium-containing slurry is matched with fuel feeding, the temperature of the fluidized bed is controlled at 500 ℃ through flow adjustment, and the flue gas temperature is controlled at 200 ℃;
(4) Cyclone dust collection system: the cyclone dust collection system consists of a cyclone dust collector, a rotary discharging valve and a high vanadium slag tank, and is used for separating substances generated after reaction, the separated solid phase high vanadium slag enters the slag tank for collection, and the separated gas-phase titanium tetrachloride enters the leaching system for washing for 20min, so as to collect the high vanadium slag;
(5) After the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby;
(6) And after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
Example 2
(1) Starting a circulating pump of a leaching system, spraying titanium tetrachloride into a leaching tower, establishing a leaching system circulation, wherein the leaching system is used for collecting the gaseous titanium tetrachloride generated by a fluidized bed, the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid matters and returns to the fluidized bed again through a mud return pipeline, the titanium tetrachloride solid matters collected by the leaching tower 2 are controlled to be 0.1g, the titanium tetrachloride solid matters can return to a refining system again for purification, a heat exchanger is used for cooling the titanium tetrachloride, and the leached tail gas enters a tail gas system for washing and is discharged after reaching standards;
(2) Feeding system: adding the fluidized material and the fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 18 hours, establishing a material layer, wherein a feeding system consists of a fluidized material bin, a fuel material bin, a metering screw and a mixed feeder and is used for conveying the fluidized material and the fuel into the fluidized bed reactor, wherein the fluidized material bin is a fluidized material, zirconium bead inert materials are selected, and the inert materials do not participate in the reaction and are used for establishing and heat accumulating of the fluidized bed layer; the fuel bin material is fuel, and can be selected from petroleum coke solid fuel for the heat supply of the fluidized bed reactor;
(3) After the temperature in the bed reaches 500 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, wherein the fluidized bed reactor consists of a fluidized bed reactor body, an air pipeline and a slurry adjusting pipeline, the air pipeline is used for providing gas required by fluidization of the fluidized bed and oxygen required by reaction, the slurry adjusting pipeline consists of a refined slurry pipeline and a circulating slurry pipeline, the refined slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed, the vanadium-containing slurry is matched with fuel feeding, the temperature of the fluidized bed is controlled at 700 ℃ through flow adjustment, and the flue gas temperature is controlled at 300 ℃;
(4) Cyclone dust collection system: the cyclone dust collection system consists of a cyclone dust collector, a rotary discharging valve and a high vanadium slag tank, and is used for separating substances generated after reaction, the separated solid phase high vanadium slag enters the slag tank for collection, and the separated gas-phase titanium tetrachloride enters the leaching system for washing for 40min, so as to collect the high vanadium slag;
(5) After the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby;
(6) And after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
Example 3
(1) Starting a circulating pump of a leaching system, spraying titanium tetrachloride into a leaching tower, establishing a leaching system circulation, wherein the leaching system is used for collecting the gaseous titanium tetrachloride generated by a fluidized bed, the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid matters and returns to the fluidized bed again through a mud return pipeline, the titanium tetrachloride solid matters collected by the leaching tower 2 are controlled to be 0.505g, the titanium tetrachloride solid matters can return to a refining system again for purification, a heat exchanger is used for cooling the titanium tetrachloride, and the leached tail gas enters a tail gas system for washing and is discharged after reaching standards;
(2) Feeding system: adding the fluidized material and the fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 14 hours, and establishing a material layer, wherein a feeding system consists of a fluidized material bin, a fuel material bin, a metering screw and a mixed feeder and is used for conveying the fluidized material and the fuel into the fluidized bed reactor, wherein the fluidized material bin is a fluidized material, quartz sand inert materials can be selected, and the inert materials do not participate in the reaction and are used for establishing and heat accumulating of the fluidized bed layer; the fuel bin material is fuel, and can be selected from petroleum coke solid fuel for the heat supply of the fluidized bed reactor;
(3) After the temperature in the bed reaches 450 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, wherein the fluidized bed reactor consists of a fluidized bed reactor body, an air pipeline and a slurry adjusting pipeline, the air pipeline is used for providing gas required by fluidization of the fluidized bed and oxygen required by reaction, the slurry adjusting pipeline consists of a refined slurry pipeline and a circulating slurry pipeline, the refined slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed, the vanadium-containing slurry is matched with fuel feeding, the temperature of the fluidized bed is controlled at 600 ℃ through flow adjustment, and the flue gas temperature is controlled at 250 ℃;
(4) Cyclone dust collection system: the cyclone dust collection system consists of a cyclone dust collector, a rotary discharging valve and a high vanadium slag tank, and is used for separating substances generated after reaction, the separated solid phase high vanadium slag enters the slag tank for collection, and the separated gas-phase titanium tetrachloride enters the leaching system for washing for 30min, so as to collect the high vanadium slag;
(5) After the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby;
(6) And after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
Example 4
(1) Starting a circulating pump of a leaching system, spraying titanium tetrachloride into a leaching tower, establishing a leaching system circulation, wherein the leaching system is used for collecting the gaseous titanium tetrachloride generated by a fluidized bed, the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid matters and returns to the fluidized bed again through a mud return pipeline, the titanium tetrachloride solid matters collected by the leaching tower 2 are controlled to be 0.01g, the titanium tetrachloride solid matters can return to a refining system again for purification, a heat exchanger is used for cooling the titanium tetrachloride, and the leached tail gas enters a tail gas system for washing and is discharged after reaching standards;
(2) Feeding system: adding the fluidized material and the fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 18 hours, establishing a material layer, wherein a feeding system consists of a fluidized material bin, a fuel material bin, a metering screw and a mixed feeder and is used for conveying the fluidized material and the fuel into the fluidized bed reactor, wherein the fluidized material bin is a fluidized material, zirconium bead inert materials are selected, and the inert materials do not participate in the reaction and are used for establishing and heat accumulating of the fluidized bed layer; the fuel bin material is fuel, and can be selected from petroleum coke solid fuel for the heat supply of the fluidized bed reactor;
(3) After the temperature in the bed reaches 500 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, wherein the fluidized bed reactor consists of a fluidized bed reactor body, an air pipeline and a slurry adjusting pipeline, the air pipeline is used for providing gas required by fluidization of the fluidized bed and oxygen required by reaction, the slurry adjusting pipeline consists of a refined slurry pipeline and a circulating slurry pipeline, the refined slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed, the vanadium-containing slurry is matched with fuel feeding, the temperature of the fluidized bed is controlled at 700 ℃ through flow adjustment, and the flue gas temperature is controlled at 300 ℃;
(4) Cyclone dust collection system: the cyclone dust collection system consists of a cyclone dust collector, a rotary discharging valve and a high vanadium slag tank, and is used for separating substances generated after reaction, the separated solid phase high vanadium slag enters the slag tank for collection, and the separated gas-phase titanium tetrachloride enters the leaching system for washing for 30min, so as to collect the high vanadium slag;
(5) After the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby;
(6) And after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
Example 5
(1) Starting a circulating pump of a leaching system, spraying titanium tetrachloride into a leaching tower, establishing a leaching system circulation, wherein the leaching system is used for collecting the gaseous titanium tetrachloride generated by a fluidized bed, the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid matters and returns to the fluidized bed again through a mud return pipeline, the titanium tetrachloride solid matters collected by the leaching tower 2 are controlled to be 0.1g, the titanium tetrachloride solid matters can return to a refining system again for purification, a heat exchanger is used for cooling the titanium tetrachloride, and the leached tail gas enters a tail gas system for washing and is discharged after reaching standards;
(2) Feeding system: adding the fluidized material and the fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 14 hours, and establishing a material layer, wherein a feeding system consists of a fluidized material bin, a fuel material bin, a metering screw and a mixed feeder and is used for conveying the fluidized material and the fuel into the fluidized bed reactor, wherein the fluidized material bin is a fluidized material, quartz sand inert materials can be selected, and the inert materials do not participate in the reaction and are used for establishing and heat accumulating of the fluidized bed layer; the fuel bin material is fuel, and can be selected from petroleum coke solid fuel for the heat supply of the fluidized bed reactor;
(3) After the temperature in the bed reaches 450 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, wherein the fluidized bed reactor consists of a fluidized bed reactor body, an air pipeline and a slurry adjusting pipeline, the air pipeline is used for providing gas required by fluidization of the fluidized bed and oxygen required by reaction, the slurry adjusting pipeline consists of a refined slurry pipeline and a circulating slurry pipeline, the refined slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed, the vanadium-containing slurry is matched with fuel feeding, the temperature of the fluidized bed is controlled at 600 ℃ through flow adjustment, and the flue gas temperature is controlled at 250 ℃;
(4) Cyclone dust collection system: the cyclone dust collection system consists of a cyclone dust collector, a rotary discharging valve and a high vanadium slag tank, and is used for separating substances generated after reaction, the separated solid phase high vanadium slag enters the slag tank for collection, and the separated gas-phase titanium tetrachloride enters the leaching system for washing for 20min, so as to collect the high vanadium slag;
(5) After the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby;
(6) And after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
Comparative example 1
(1) Starting a circulating pump of a leaching system, spraying titanium tetrachloride into a leaching tower, establishing a leaching system circulation, wherein the leaching system is used for collecting the gaseous titanium tetrachloride generated by a fluidized bed, the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid matters and returns to the fluidized bed again through a mud return pipeline, the titanium tetrachloride solid matters collected by the leaching tower 2 are controlled to be 0.1g, the titanium tetrachloride solid matters can return to a refining system again for purification, a heat exchanger is used for cooling the titanium tetrachloride, and the leached tail gas enters a tail gas system for washing and is discharged after reaching standards;
(2) Feeding system: adding the fluidized material and the fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 14 hours, and establishing a material layer, wherein a feeding system consists of a fluidized material bin, a fuel material bin, a metering screw and a mixed feeder and is used for conveying the fluidized material and the fuel into the fluidized bed reactor, wherein the fluidized material bin is a fluidized material, quartz sand inert materials can be selected, and the inert materials do not participate in the reaction and are used for establishing and heat accumulating of the fluidized bed layer; the fuel bin material is fuel, and can be selected from petroleum coke solid fuel for the heat supply of the fluidized bed reactor;
(3) After the temperature in the bed reaches 450 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, wherein the fluidized bed reactor consists of a fluidized bed reactor body, an air pipeline and a slurry adjusting pipeline, the air pipeline is used for providing gas required by fluidization of the fluidized bed and oxygen required by reaction, the slurry adjusting pipeline consists of a refined slurry pipeline and a circulating slurry pipeline, the refined slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed, the vanadium-containing slurry is matched with fuel feeding, the temperature of the fluidized bed is controlled at 600 ℃ through flow adjustment, and the flue gas temperature is controlled at 250 ℃;
(4) Cyclone dust collection system: the cyclone dust collection system consists of a cyclone dust collector, a rotary discharging valve and a high vanadium slag tank, and is used for separating substances generated after reaction, the separated solid phase high vanadium slag enters the slag tank for collection, and the separated gas-phase titanium tetrachloride enters the leaching system for washing for 20min, so as to collect the high vanadium slag;
the preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (6)
1. A method for preparing high vanadium slag by treating vanadium-containing slurry by a fluidized bed, which is characterized by comprising the following steps:
(1) Starting a circulating pump of the leaching system, spraying titanium tetrachloride into the leaching tower, and establishing the circulation of the leaching system;
(2) Feeding system: adding the fluidized material and fuel into a fluidized bed reactor through a metering screw, introducing air for reaction for 10-18h, and establishing a material layer;
(3) After the temperature in the bed reaches 400-500 ℃, circulating slurry and refined vanadium-containing slurry are introduced into a fluidized bed reactor, the temperature of the fluidized bed is controlled at 500-700 ℃ through flow regulation, and the temperature of flue gas is controlled at 200-300 ℃;
(4) Cyclone dust collection system: alternately starting a cyclone blanking rotary valve 1 and a rotary valve 2, and collecting high vanadium slag;
(5) After the liquid level of the condensate collecting tank reaches the upper limit, conveying titanium tetrachloride to a crude titanium tetrachloride storage tank of a refining system for standby;
(6) And after the material level of the high vanadium slag tank reaches the upper limit, replacing the high vanadium slag tank to continuously collect the high vanadium slag.
2. The method for preparing high vanadium slag by treating vanadium-containing slurry with fluidized bed according to claim 1, wherein the leaching system in (1) is used for collecting the gas-phase titanium tetrachloride generated by the fluidized bed, wherein the titanium tetrachloride collected by the leaching tower 1 contains a small amount of vanadium-containing solid phase matters, the solid phase matters are returned to the fluidized bed through a mud return pipeline, the solid phase matters of the titanium tetrachloride collected by the leaching tower 2 are controlled to be 0.01-0.1g, the solid phase matters can be returned to the refining system again for purification, the heat exchanger is used for cooling the titanium tetrachloride, and the tail gas after leaching enters the tail gas system for washing and is discharged after reaching standards.
3. The method for preparing high vanadium slag by treating vanadium-containing slurry with fluidized bed according to claim 1, wherein the feeding system in (2) comprises a fluidization bin, a fuel bin, a metering screw and a mixing feeder for delivering the fluidization material and the fuel into the fluidized bed reactor.
4. The method for preparing high vanadium slag by treating vanadium-containing slurry with a fluidized bed according to claim 1, wherein the fluidized material in the fluidized material bin in the step (2) is fluidized material, and quartz sand or zirconium bead inert material is selected, and the inert material does not participate in the reaction and is used for establishing and heat accumulating a fluidized bed layer; the material of the fuel bin is fuel, and can be coal or petroleum coke solid fuel for the heat supply of the fluidized bed reactor.
5. The method for preparing high vanadium slag by treating vanadium-containing slurry with fluidized bed according to claim 1, wherein the fluidized bed reactor in (3) comprises a fluidized bed reactor body, an air pipeline and a slurry regulating pipeline, wherein the air pipeline is used for providing gas required for fluidization of the fluidized bed and oxygen required for reaction, and the slurry regulating pipeline comprises a refining slurry pipeline and a circulating slurry pipeline, wherein the refining slurry pipeline is used for introducing vanadium-containing slurry produced by refining titanium tetrachloride into the fluidized bed and is matched with fuel feeding.
6. The method for preparing high-vanadium slag by treating vanadium-containing slurry with a fluidized bed according to claim 1, wherein the cyclone dust collection system in (4) consists of a cyclone dust collector, a rotary blanking valve and a high-vanadium slag tank, and is used for separating substances generated after reaction, the separated solid-phase high-vanadium slag enters the slag tank to be collected, and the separated gas-phase titanium tetrachloride enters the leaching system to be washed for 20-40min.
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