CN111892085A - Vanadium trioxide preparation system and preparation method - Google Patents
Vanadium trioxide preparation system and preparation method Download PDFInfo
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- CN111892085A CN111892085A CN202010704963.5A CN202010704963A CN111892085A CN 111892085 A CN111892085 A CN 111892085A CN 202010704963 A CN202010704963 A CN 202010704963A CN 111892085 A CN111892085 A CN 111892085A
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- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- 238000001035 drying Methods 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000007086 side reaction Methods 0.000 claims abstract description 15
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 14
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 14
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008117 stearic acid Substances 0.000 claims abstract description 14
- 238000005243 fluidization Methods 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 23
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 13
- 238000010517 secondary reaction Methods 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003034 coal gas Substances 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000002829 reductive effect Effects 0.000 abstract description 5
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000013021 overheating Methods 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 description 16
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 9
- 238000006722 reduction reaction Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 239000011541 reaction mixture Substances 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 2
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 description 2
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 1
- 229910001199 N alloy Inorganic materials 0.000 description 1
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910001617 alkaline earth metal chloride Inorganic materials 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A vanadium trioxide preparation system comprises a fluidized reactor, a feeding device, a heating system, an air blast cooling system, a heat exchanger and a discharging device; the feeding device is positioned at the upper part of the feeding end of the fluidized reactor, the heating system adjusts the temperature of the fluidized reactor, a drying zone, a pre-reaction zone, a main reaction zone and an auxiliary reaction zone are sequentially arranged in a cavity of the fluidized reactor from top to bottom, a first air inlet is arranged on the cavity of the drying zone, an air outlet is arranged on the cavity of the main reaction zone, and the blast cooling system is connected with the auxiliary reaction zone of the fluidized reactor through a heat exchanger. The preparation method comprises the steps of preheating the fluidization reactor, uniformly mixing ammonium polyvanadate and stearic acid, adding, controlling the reaction temperature of the fluidization reactor, introducing reducing gas into the side reaction zone from the lower part of the fluidization reactor for reaction, cooling the obtained product, and separating to obtain vanadium trioxide. The temperature is uniformly distributed according to regions in the reaction process, the local overheating phenomenon is avoided, the fluidization is uniform, the reaction time is short, and the energy consumption and the manufacturing cost are reduced.
Description
Technical Field
The invention relates to a vanadium trioxide preparation system and a preparation method, and belongs to the technical field of chemical production.
Background
The vanadium oxide is mainly used for producing alloy and ceramic sealThe dye can be used in industries such as metallurgy, electronics, dye, energy, chemical engineering and the like, such as dye colorant, all-vanadium redox flow battery electrolyte, sulfuric acid, catalyst of petrochemical engineering and the like. The vanadium oxide is mainly vanadium pentoxide (V)2O5) Vanadium (V) oxide2O3) And vanadium dioxide (VO)2) And the preparation process of different oxides is different. Vanadium trioxide is an ideal raw material for producing vanadium-nitrogen alloy and ferrovanadium alloy, at present, the common method for producing vanadium trioxide is to use ammonium metavanadate, ammonium polyvanadate, vanadium pentoxide and the like as raw materials, and reduce the raw materials by using reductive gases such as natural gas, coal gas, hydrogen and the like at the temperature of 800-.
CN103922404B discloses a method for preparing vanadium trioxide from vanadium pentoxide, which comprises the steps of uniformly mixing vanadium pentoxide and carbon powder according to a molar ratio of 2: 1; pressing the mixed raw materials into a material block, and covering carbon powder on the material block; and firing the formed material block at 950-1050 ℃ for 3-5h to obtain vanadium trioxide. The reduction temperature of the invention is above 900 ℃, the energy consumption is higher, and the invention is not beneficial to popularization. CN103695954B discloses a method for preparing vanadium trioxide by direct electrolysis of vanadate, which comprises heating vanadate serving as a raw material and alkali metal or alkaline earth metal chloride serving as molten salt under the atmosphere of nitrogen or argon to 150-250 ℃, keeping the temperature for 12-24 h to remove water in the molten salt, heating to 500-1000 ℃ for electrolysis, wherein the cell voltage is 2.5-5.0V, the electrolysis time is 3-12 h, and obtaining a product vanadium trioxide product at the lower part of a cathode. However, the electrolytic preparation process also has the problem of high energy consumption. CN106006736A discloses a method for preparing vanadium trioxide from vanadium-containing solution by using hydrogen, wherein the hydrogen and vanadium concentration is more than 6g/L, and the hydrogen ion concentration is 10-4-10-14The vanadium-containing solution reacts for more than 1 hour in a high-temperature high-pressure reaction device at the temperature of between 50 and 300 ℃ and under the partial pressure of hydrogen of more than 1MPa, and a vanadium trioxide product is obtained. The method has the defects of harsh reaction conditions and incomplete reduction reaction, and meanwhile, a large amount of sodium hydroxide solution with low concentration is produced as a byproduct, so that the recycling is difficult and the method needs to be carried outAnd adopting other methods for processing.
In view of the above, it is desirable to develop a vanadium trioxide preparation system and a preparation method thereof, which have short production process, low energy consumption, no ammonia nitrogen wastewater and efficient reduction reaction.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a vanadium trioxide preparation system and a preparation method with short production flow and low energy consumption.
In order to achieve the purpose, the invention adopts the technical scheme that:
a vanadium trioxide preparation system comprises a fluidized reactor, a feeding device, a heating system, an air blast cooling system, a heat exchanger and a discharging device; the feeding device is positioned at the upper part of the feeding end of the fluidized reactor, the heating system adjusts the temperature of the fluidized reactor through electric heating or coal gas heating, a drying zone, a pre-reaction zone, a main reaction zone and an auxiliary reaction zone are sequentially arranged in a cavity of the fluidized reactor from top to bottom, a first air inlet is arranged on the cavity of the drying zone, an air outlet is arranged on the cavity of the main reaction zone, and the blast cooling system is connected with the auxiliary reaction zone of the fluidized reactor through a heat exchanger.
Preferably, the reactor further comprises a PRISM membrane separation device, a second air inlet is arranged on the cavity of the secondary reaction zone, the inlet end of the PRISM membrane separation device is connected with the air outlet pipeline on the main reaction zone, and the two outlet ends of the PRISM membrane separation device are respectively connected with the first air inlet and the second air inlet pipeline.
Preferably, the outlet end of the forced air cooling system is connected with the inlet end of the heat exchanger, and the outlet end of the heat exchanger is communicated with the secondary reaction zone.
The invention also provides a preparation method of vanadium trioxide, which is prepared by using the vanadium trioxide preparation system and comprises the following steps:
a. preheating a fluidized reactor at the preheating temperature of 60-100 ℃, and introducing inert gas to replace air in the fluidized reactor;
b. uniformly mixing ammonium polyvanadate and stearic acid, and adding the mixture into a fluidization reactor through a feeding device, wherein the mixing proportion is that the stearic acid accounts for 0.01-2% and the balance is ammonium polyvanadate according to the weight percentage;
c. controlling the temperature of a drying zone of the fluidized reactor to be 80-100 ℃, the temperature of a pre-reaction zone to be 200-450 ℃, the temperature of a main reaction zone to be 600-650 ℃, and the temperature of a side reaction zone to be 600-450 ℃ by a heating system;
d. the reducing gas is introduced into the side reaction zone from the lower part of the fluidized reactor to react;
e. and after the reaction is finished, cooling the obtained product, and carrying out gas-solid separation to obtain vanadium trioxide.
Preferably, the vanadium trioxide is cooled to room temperature after the reducing gas passes through the blast cooling system, and the vanadium trioxide is output through the discharging device.
Preferably, in the step d, the reducing gas passes through a blast cooling system, then passes through a heat exchanger to be heated to 500-700 ℃, and then flows into a secondary reaction zone in the fluidized reactor.
Preferably, after the PRISM membrane separation device treats the gas generated by the reaction, the inert gas returns to the drying zone through the first gas inlet for reaction, and the reducing gas returns to the side reaction zone through the second gas inlet for reaction;
preferably, the inert gas is nitrogen and the reducing gas is hydrogen.
Preferably, the retention time of the added materials ammonium polyvanadate and stearic acid in the drying zone is controlled to be 50-180 min, the retention time in the pre-reaction zone is controlled to be 20-30 min, the retention time in the main reaction zone is controlled to be 10-20 min, and the retention time in the secondary reaction zone is controlled to be 5-20 min;
in the step d, the flow rate of the ammonium polyvanadate reducing gas is 20m per 1t of the ammonium polyvanadate3/h~100 m3H, preferably 30m3/h~80 m3/h。
The principle of the invention is that ammonium polyvanadate with the moisture content of less than 40 percent is mixed with an auxiliary agent stearic acid, then dehydration drying is carried out at the temperature of 80-100 ℃, and reducing gas H is introduced into the mixture after drying at the reaction temperature of 550-600 DEG C2Reacting to generate vanadium trioxide and ammonia gas, and returning the hydrogen and nitrogen generated after the ammonia gas is decomposed to the systemThe system continues to react, wherein the chemical reaction involved is:
(NH4) 2V6O16+6H2= 3V2O3+7H2O +2NH3
2NH3= 3H2+N2
compared with the existing vanadium trioxide production method, the method has the advantages of low reaction temperature, better heat transfer effect, reaction time shortening, energy saving by more than 30 percent and production cost reduction. The stearic acid added as an auxiliary agent is a surfactant, so that wall adhesion in the drying process of the ammonium polyvanadate can be prevented, and the wall bonding problem in the traditional process is effectively avoided.
Compared with the prior art, the invention has the advantages that:
(1) compared with the traditional process, the reaction of the process is carried out in a subarea manner, so that the phenomenon of material wall formation caused by local overheating in the drying process is avoided, and a better heat transfer effect is realized by adopting a fluidization manner;
(2) the traditional process has the reduction temperature of 600-900 ℃, the reaction time of about 20min, the reduction temperature of 550-600 ℃ and the reduction time of 7-10 min, so that the reaction time is greatly shortened, and the reaction temperature is reduced;
(3) traditional processes require about 92m for reducing the ammonium polyvanadate, and the process requires about 60 m for reducing the ammonium polyvanadate for treating 1 ton of ammonium polyvanadate; the energy is saved by more than 30%, and the production cost is reduced;
(4) through detection, the grade of the vanadium trioxide product produced by the method is up to more than 67 percent;
in addition, in the preferred scheme of the invention, hydrogen and nitrogen generated in the production process are returned to the system for continuous use, so that the production cost is reduced, and the method has important significance for reducing the energy consumption of the whole process.
Drawings
FIG. 1 is a schematic structural view of one embodiment of a vanadium trioxide production system according to the present invention;
FIG. 2 is a process flow diagram of one embodiment of the method for preparing vanadium trioxide according to the invention.
Labeled as: 1. the device comprises a discharging device, 2 a blast cooling system, 3 a heat exchanger, 4 a second air inlet, 5 a secondary reaction zone, 6a main reaction zone, 7 a PRISM membrane separation device, 8 a first air inlet, 9 a heating system, 10 a pre-reaction zone, 11 a drying zone, 12 a fluidization reactor, 13 a feeding device and 14 an air outlet.
Detailed Description
The technical solution of the present invention is further described in detail by embodiments with reference to the accompanying drawings.
A vanadium trioxide preparation system comprises a fluidized reactor 12, a feeding device 13, a heating system 9, a blast cooling system 2, a heat exchanger 3, a PRISM membrane separation device 7, a first air inlet 8, a second air inlet 4 and a discharging device 1, wherein the first air inlet 8, the second air inlet 4 and the discharging device are arranged on a drying area cavity; the feeding device 13 is a spiral feeding device, the type gy-108 is installed at the upper part of the feeding end of the fluidized reactor 12, the fluidized reactor 12 is a fluidized bed, a cavity is sequentially divided into a drying zone 11, a pre-reaction zone 10, an auxiliary reaction zone 5 and a main reaction zone 6 from top to bottom, and a heating system 9 controls the temperature of the drying zone 11, the pre-reaction zone 10, the auxiliary reaction zone 5 and the main reaction zone 6 through known electric heating; 2m for blast cooling system2In the traditional blast circular cooler, the pitch diameter of a circular cooler is 400mm, the material handling capacity is 2t/h, and the traditional blast circular cooler is connected with a fluidized reactor 12 through a heat exchanger 3; the secondary reaction zone 5 and the main reaction zone 6 are respectively connected with a PRISM membrane separation device 7 through pipelines, wherein the inlet end of the PRISM membrane separation device 7 is connected with a gas outlet 14 on the main reaction zone 6 through a pipeline, namely, after gas generated by the secondary reaction zone 5 and the main reaction zone 6 is separated through the PRISM membrane separation device 7, nitrogen returns to the drying zone 11 through the first gas inlet 8 for reaction, and hydrogen returns to the secondary reaction zone 5 through the second gas inlet 4 for reaction; the reducing gas passes through the blast cooling system 2 and then cools the vanadium trioxide to room temperature, and the gas is heated by the heat exchanger 3 and then enters the reaction device for reaction.
In examples 1 to 6 of the method for producing vanadium trioxide of the present invention, the production was carried out by using the above-mentioned system for producing vanadium trioxide.
Example 1:
the preparation method comprises the following steps:
a. preheating the fluidized reactor to 100 ℃, and introducing nitrogen to replace air in the fluidized reactor;
b, adding the uniformly mixed ammonium polyvanadate and stearic acid into a fluidized reactor according to a dry basis of 1t/h by using a feeding device, wherein the mixing proportion is 2% by weight and 98% by weight;
c. controlling the temperature of a drying zone of the fluidized reactor at 91 ℃ through a heating system, and keeping the material for 120 min; the temperature of the pre-reaction zone is controlled to be 430 ℃, and the material retention time is 25 min; the temperature of the main reaction zone is 600 ℃, and the material retention time is 15 min; the temperature of the side reaction zone is 550 ℃, and the material retention time is 10 min;
d. after the gas generated in the reaction process is collected and processed, nitrogen enters a drying area through a first gas inlet (8), hydrogen returns to a side reaction area 5 through a second gas inlet 4 for reaction, and the hydrogen flow is controlled to be 60 m3And h, allowing the reaction product to pass through a blast cooling system, allowing the heat exchange temperature to reach 580 ℃ to enter a reaction system for reaction, cooling the reaction product to room temperature, separating by using a cyclone separator to obtain vanadium trioxide, and outputting the vanadium trioxide through a discharging device.
Example 2:
the preparation method comprises the following steps:
a. preheating the fluidized reactor to 90 ℃, and introducing nitrogen to replace air in the fluidized reactor;
b, adding the uniformly mixed ammonium polyvanadate and stearic acid into a fluidized reactor according to a dry basis of 1t/h by a feeding device, wherein the mixing proportion is 1 percent by weight and 99 percent by weight;
c. controlling the temperature of a drying zone of the fluidized reactor at 100 ℃ by a heating system, and keeping the material for 80 min; the temperature of the pre-reaction zone is controlled to be 350 ℃, and the material retention time is 22 min; the temperature of the main reaction zone is 630 ℃, and the material retention time is 18 min; the temperature of the side reaction zone is 450 ℃, and the material retention time is 5 min;
d. after the gas generated in the reaction process is collected and treated, the nitrogen enters the drying device through a first gas inlet (8)Hydrogen returns to the side reaction zone 5 through the second gas inlet 4 to react, and the hydrogen flow is controlled to be 45 m3And h, allowing the reaction mixture to pass through a blast cooling system, allowing the heat exchange temperature to reach 500 ℃ and enter a reaction system for reaction, cooling the reaction mixture to room temperature, separating by using a cyclone separator to obtain vanadium trioxide, and outputting the vanadium trioxide through a discharging device.
Example 3:
the preparation method comprises the following steps:
a. preheating a fluidization reactor at 60 ℃, and introducing nitrogen to replace air in the fluidization reactor;
b, adding the uniformly mixed ammonium polyvanadate and stearic acid into a fluidized reactor according to a dry basis of 1t/h by using a feeding device, wherein the mixing proportion is 0.01 percent by weight and 99.99 percent by weight;
c. controlling the temperature of a drying zone of the fluidized reactor at 80 ℃ by a heating system, and keeping the material for 180 min; the temperature of the pre-reaction zone is controlled at 200 ℃, and the material retention time is 30 min; the temperature of the main reaction zone is 650 ℃, and the material retention time is 10 min; the temperature of the side reaction zone is 600 ℃, and the material retention time is 20 min;
d. after the gas generated in the reaction process is collected and processed, nitrogen enters a drying area through a first gas inlet (8), hydrogen returns to a side reaction area 5 through a second gas inlet 4 for reaction, and the hydrogen flow is controlled to be 20m3And h, allowing the reaction mixture to pass through a blast cooling system, allowing the heat exchange temperature to reach 700 ℃ and enter a reaction system for reaction, cooling the reaction mixture to room temperature, separating by using a cyclone separator to obtain vanadium trioxide, and outputting the vanadium trioxide through a discharging device.
Example 4:
the preparation method comprises the following steps:
a. preheating a fluidization reactor at 85 ℃, and introducing nitrogen to replace air in the fluidization reactor;
b, adding the uniformly mixed ammonium polyvanadate and stearic acid into a fluidized reactor according to a dry basis of 1t/h by a feeding device, wherein the mixing proportion is 1.50 percent of stearic acid and 98.50 percent of ammonium polyvanadate according to the weight percentage content;
c. controlling the temperature of a drying zone of the fluidized reactor at 95 ℃ by a heating system, and keeping the material for 50 min; the temperature of the pre-reaction zone is controlled to be 450 ℃, and the material retention time is 20 min; the temperature of the main reaction zone is 620 ℃, and the material retention time is 20 min; the temperature of the side reaction zone is 500 ℃, and the material retention time is 15 min;
d. after the gas generated in the reaction process is collected and processed, nitrogen enters a drying area through a first gas inlet (8), hydrogen returns to a side reaction area 5 through a second gas inlet 4 for reaction, and the hydrogen flow is controlled to be 100 m3And h, passing through a blast cooling system, allowing the heat exchange temperature to reach 620 ℃, allowing the reaction product to enter a reaction system for reaction, cooling the reaction product to room temperature, separating the reaction product by using a cyclone separator to obtain vanadium trioxide, and outputting the vanadium trioxide through a discharging device.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A vanadium trioxide preparation system is characterized by comprising a fluidization reactor (12), a feeding device (13), a heating system (9), an air blast cooling system (2), a heat exchanger (3) and a discharging device (1); the feeding device (13) is positioned at the upper part of the feeding end of the fluidized reactor (12), the heating system (9) adjusts the temperature of the fluidized reactor (12) through electric heating or coal gas heating, a drying zone (11), a pre-reaction zone (10), a main reaction zone (6) and an auxiliary reaction zone (5) are sequentially arranged in a cavity of the fluidized reactor (12) from top to bottom, a first air inlet (8) is arranged on the cavity of the drying zone, an air outlet (14) is arranged on the cavity of the main reaction zone (6), and the blast cooling system (2) is connected with the auxiliary reaction zone (5) of the fluidized reactor (12) through a heat exchanger (3).
2. The vanadium trioxide preparation system according to claim 1, characterized in that the composition further comprises a PRISM membrane separation device (7), a second gas inlet (4) is arranged on the cavity of the secondary reaction zone (5), the inlet end of the PRISM membrane separation device (7) is connected with the gas outlet (14) of the primary reaction zone (6) through a pipeline, and the two outlet ends of the PRISM membrane separation device (7) are respectively connected with the first gas inlet (8) and the second gas inlet (4) through pipelines.
3. The vanadium trioxide preparation system according to claim 1 or 2, characterized in that the outlet end of the blast cooling system (2) is connected with the inlet end of the heat exchanger (3), and the outlet end of the heat exchanger (3) is communicated with the secondary reaction zone (5).
4. A method for producing vanadium trioxide, characterized by using the vanadium trioxide production system according to any one of claims 1 to 3, comprising the steps of:
a. preheating the fluidized reactor at the preheating temperature of 60-100 ℃, and introducing inert gas to replace air in the fluidized reactor;
b. after ammonium polyvanadate and stearic acid are uniformly mixed, the mixture is added into a fluidization reactor (12) through a feeding device (13), the mixing proportion is that the stearic acid accounts for 0.01 to 2 percent and the rest is ammonium polyvanadate according to the weight percentage;
c. controlling the temperature of a drying zone (11) of the fluidized reactor to be 80-100 ℃ through a heating system (9), controlling the temperature of a pre-reaction zone (10) to be 200-450 ℃, controlling the temperature of a main reaction zone (6) to be 600-650 ℃, and controlling the temperature of a side reaction zone (5) to be 600-450 ℃;
d. the reducing gas is introduced into the side reaction zone from the lower part of the fluidized reactor to react;
e. and after the reaction is finished, cooling the obtained product, and performing gas-solid separation to obtain vanadium trioxide.
5. The preparation method of vanadium trioxide according to claim 4, characterized in that the vanadium trioxide is cooled to room temperature after the reducing gas passes through the blast cooling system (2), and the vanadium trioxide is output through a discharging device.
6. The method for preparing vanadium trioxide according to claim 5, characterized in that in the step d, the reducing gas passes through a blast cooling system (2), then passes through a heat exchanger (3) to be heated to 500-700 ℃, and then enters a secondary reaction zone (5) in a fluidized reactor.
7. The method for producing vanadium trioxide according to claim 6, wherein the vanadium trioxide is produced by the method of the present invention
After the PRISM membrane separation device (7) treats the gas generated by the reaction, the inert gas returns to the drying zone (11) through the first gas inlet (8) for reaction, and the reducing gas returns to the side reaction zone (5) through the second gas inlet (4) for reaction.
8. The method for preparing vanadium trioxide according to claim 7, wherein the inert gas is nitrogen and the reducing gas is hydrogen.
9. The method for preparing vanadium trioxide according to claim 6, wherein the added materials ammonium polyvanadate and stearic acid are kept in the drying zone for 50-180 min, the pre-reaction zone is kept for 20-30 min, the main reaction zone is kept for 10-20 min, and the secondary reaction zone is kept for 5-20 min.
10. The method according to claim 9, wherein the flow rate of the reducing gas is 20m per 1t of ammonium polyvanadate3/h~100 m3/h 。
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