CN111592041B - Melting furnace and method for smelting vanadium pentoxide by using same - Google Patents
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Abstract
The invention discloses a melting furnace and a method for smelting vanadium pentoxide by using the melting furnace, and belongs to the technical field of metallurgy. The invention provides a method for smelting vanadium pentoxide by using a melting furnace to make up for the defects in the prior art, which comprises the following steps: adding vanadium-containing materials into the melting furnace through a feeding port, and piling the vanadium-containing materials into two inclined triangular material piles leading to a discharge port; firstly, controlling the temperature to reach 300-550 ℃, and drying and dehydrating; then controlling the temperature to 550-650 ℃ for deamination and dehydration; finally, controlling the temperature to reach 676-800 ℃, carrying out vanadium oxidation and melting, and melting out the melted materials. The invention realizes melting and discharging by improving the melting furnace and the material distribution mode, greatly reduces the vanadium oxidation and melting temperature, effectively solves the vanadium vaporization loss in the melting process, and saves energy sources; and a continuous production mode of 'continuous feeding and continuous discharging' is realized, so that the quality of the flaky vanadium pentoxide is improved, and the production efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a novel melting furnace and a method for smelting vanadium pentoxide by using the same.
Background
The production of vanadium pentoxide by melting furnace mainly includes three stages of APV dehydration, deaminization and melting cast sheet. The Xichang steel vanadium products division of Pan Steel group adopts the existing 2 seats of 20m 2 The melting furnace, the present melting furnace cloth mode mainly has impartial cloth, 1221 cloth and 2112 cloth mode: the equal distribution mode is that the materials are equally fed according to 4 feed ports, the fed materials form an equal distribution mode in the molten pool, and because of the equal distribution, the furnace bottom basically forms a horizontal plane, molten iron at two ends of the molten pool slowly flows, and the production efficiency is low; 1221 material distribution mode is to reduce 1# and 4# feeding amount, improve 2# and 3# feeding amount, the 2# and 3# feeding amount is 2 times of 1# and 4# feeding amount, form a convex surface in the molten pool, molten iron melted in the middle part is easy to flow to two ends of the molten pool, when the liquid level of the molten pool falls to a certain height, the materials at two ends flow back again, the molten iron stays in the molten pool for a long time, conditions are created for side reaction, grade is reduced, and vanadium loss is increased; 2112 the material distribution mode is the best at present, which reduces the feeding amount of No. 2 and No. 3, increases the feeding amount of No. 1 and No. 4, the feeding amount of No. 1 and No. 4 is 2 times of the feeding amount of No. 2 and No. 3,the concave surface is formed in the molten pool, materials at two ends of the melting furnace gradually flow to the middle part after being melted and smoothly flow out of the iron outlet, so that the problems of backflow, slow flow and the like of molten iron in the molten pool are avoided, the occurrence of side reactions in the melting process is reduced, and the production efficiency and the product quality are ensured.
However, the processes all adopt 'single charging and single discharging', and the process for producing the vanadium pentoxide by the melting furnace is simple and rough and is divided into three stages (three stages of charging, material sealing and discharging): a charging and material enclosing stage; single charging is adopted for charging; in the '2112' material pile mode, the material is sealed into three temperature sections: 1-stage I, 1-stage II, 800-850, 3h, and III-stage III, wherein the temperature is 700-800 ℃ and 1h; discharging: smelting for 3-4h at 900-1000 ℃; the total smelting time is 8-9h. One furnace can be smelted only one furnace per one furnace, 2 seats with 20m 2 The melting furnace can only produce 7 tons of pieces of vanadium pentoxide, and the production efficiency is low; in addition, the generated vanadium has obvious vaporization phenomenon due to overhigh smelting temperature in the smelting process, and partial vaporized vanadium can be recycled only by spraying flue gas, so that the serious loss of the melting yield is caused.
There is currently no effective solution.
Disclosure of Invention
In order to make up for the defects in the prior art, the invention firstly designs a novel melting furnace which comprises two feeding ports (1), two heat sources (2) and a discharging port (4); wherein, the feed inlet (1) is positioned at the top of the furnace, the two heat sources (2) are arranged oppositely, and the discharge outlet (4) is positioned at the bottom of the furnace.
Wherein the melting furnace has a hearth area of F =20m 2 Its productivity is 380kgV 2 O 5 /m 2 ·d。
On the basis of the melting furnace, the invention further provides a method for smelting vanadium pentoxide by using the melting furnace, which comprises the following steps:
A. adding vanadium-containing materials into the melting furnace through a feed inlet (1), and stacking the vanadium-containing materials into two inclined triangular material piles (3) leading to a discharge outlet (4);
B. the temperature in the furnace is controlled to reach 300-550 ℃ through the heat source (2) to carry out drying and dehydration;
C. then controlling the temperature in the furnace to 550-650 ℃ for deamination and dehydration;
D. finally, controlling the temperature in the furnace to reach 676-800 ℃, carrying out vanadium oxidation and melting, and melting the melted materials out from the discharge hole (4).
In the method for smelting vanadium pentoxide by using the melting furnace, in order to realize a continuous production mode of 'continuous feeding and continuous discharging', a vanadium-containing material layer is supplemented to the two inclined triangular material piles through the feeding port (1) in the smelting process, and a supplemented layer is melted.
In the method for smelting vanadium pentoxide by using the melting furnace, the vanadium-containing material is ammonium polyvanadate.
In the method for smelting vanadium pentoxide by using the melting furnace, the drying and dehydrating time is 0.5-1.5 h.
In the method for smelting vanadium pentoxide by using the melting furnace, the time for deamination and dehydration is 2.5-3.5 h.
The method for smelting vanadium pentoxide by using the melting furnace further comprises the following steps: E. and after the molten material is discharged from the discharge port (4), the sheet is cast by a sheet casting device to obtain the sheet vanadium pentoxide.
The invention has the beneficial effects that:
the invention improves the melting furnace to pile the vanadium-containing material into the inclined triangular material pile leading to the discharge hole, thereby greatly reducing the vanadium oxidation and melting temperature, realizing 'melting and discharging', effectively solving the 'vanadium vaporization' loss in the melting process and saving the energy; according to the production requirement, a single-stage smelting mode of single feeding or a continuous production mode of continuous feeding and continuous discharging is adopted, the mode limitation of the original single-furnace production is changed, the quality of the flaky vanadium pentoxide is improved, the production efficiency is improved, and the continuous production mode is worthy of popularization and application.
Drawings
FIG. 1 is a schematic structural view of a melting furnace of the present invention, wherein 1 is two charging ports, 2 is two heat source burners, 3 is a stockpile, and 4 is a discharging port.
Detailed Description
The melting furnace is mainly used for producing vanadium pentoxide by three stages of APV dehydration, deamination and sheet casting melting, the operation mode in the prior art is rough, and the melting furnace is simply divided into two stages for producing vanadium pentoxide: and (3) material enclosing stage after feeding, wherein the material enclosing stage comprises three temperature sections: 1-stage I, 1-stage II, 800-850, 3h, and 950-1000 ℃ for 1h; discharging the materials, and smelting for 3-4h at 900-1000 ℃, wherein the total smelting time is 8-9h. Because the molten vanadium pentoxide stays in the furnace all the time, and the molten vanadium pentoxide is a heat release substance, heat is released continuously, the temperature in the furnace is raised due to the heat release, so that the molten vanadium pentoxide is vaporized to form vanadium steam, and the vanadium steam continuously heats the material, which is a vicious circle and aggregation of heat in the furnace; finally, the phenomena of vanadium melting, concentrated heat release, vanadium vaporization, reverse heating of vanadium vaporization heat and melting vaporization are continuously performed, so that the temperature in the furnace is increased greatly; meanwhile, only single-furnace smelting is available, and the production efficiency is very low.
On the basis of mass actual production, the chemical reaction principle of producing vanadium pentoxide by a melting furnace is deeply researched so as to optimize the process; the analysis finds that: the dehydration, deamination, ammonia decomposition, vanadium reduction, oxidation and melting vaporization reaction of the vanadium-containing material are completed in a melting furnace, and the method comprises the following specific steps:
APV dehydration deamination (temperature: 550-650 ℃):
(NH 4 ) 2 V 6 O 16 →3V 2 O 5 +2NH 3 ↑+H 2 o ↓ [ 1 ];
ammonia decomposition (conditions: nickel-based catalyst, 800-825 ℃ or iron oxide, 650 ℃ (undesired):
2NH 3 →2N 2 ↑+3H 2 ×) 2;
reduction (formula 3 temperature: about 425-450 ℃ C.; formula 4 temperature: about 674 ℃ C., undesired):
V 2 O 5 +H 2 →V 2 O 4 +H 2 o ↓ [ 3 ] of the O × (R),
V 2 O 5 +CO→V 2 O 4 +CO 2 ≈ 4;
oxidation (temperature: about 650 to 800 ℃, desired):
2V 2 O 4 +O 2 →2V 2 O 5 formula 5;
melting (temperature: 676 ℃, desired):
V 2 O 5 (s)→V 2 O 5 (l) Formula 6;
vaporization (temperature above about 900 ℃, not desired):
V 2 O 5 (l)→V 2 O 5 (g) And (7) formula.
From the above analysis, it is known that vanadium is severely vaporized at temperatures above 900 ℃, and that, since the raw material contains a very small amount of iron oxide, if vanadium stays in the melting furnace for a long time, ammonia decomposition and reduction reactions are likely to occur. In the prior art, each stage is in a high-temperature state in the smelting process, and far exceeds the melting initial theoretical temperature of 676 ℃, so that the vaporization phenomenon in the furnace is serious, smoke in the furnace is diffused, nitrogen oxides, sulfides and the like in the materials are discharged out in an overproof manner, serious environmental pollution is caused, meanwhile, serious corrosion is caused to bricks in the furnace, and SiO in the bricks is generated 2 ，A1 2 O 3 The components enter the product, which causes poor product quality and low yield. Therefore, the invention adopts the idea of melting and discharging instantly, avoids vanadium vaporization and reduction reaction, reduces corrosion of high temperature in the furnace to the brickwork and doping of brickwork components to products, and avoids generating high-temperature SO 2 Gas and the like to improve the quality and the yield of the flaky vanadium pentoxide.
Specifically, the method for smelting vanadium pentoxide by using the melting furnace comprises the following steps:
A. adding vanadium-containing materials into the melting furnace through a feeding port (1), and stacking the vanadium-containing materials into two inclined triangular material stacks (3) leading to a discharge port (4);
B. the temperature in the furnace is controlled to reach 300-550 ℃ through the heat source (2) to carry out drying and dehydration;
C. then controlling the temperature in the furnace to 550-650 ℃ for deamination and dehydration;
D. finally, controlling the temperature in the furnace to reach 676-800 ℃, carrying out vanadium oxidation and melting, and melting the melted materials from the discharge hole (4).
When the melting furnace is used for smelting vanadium pentoxide, three temperatures need to be controlled:
the first stage is as follows: removing free water (water molecules bonded by Van der Waals force on the surface of the material) and crystal water (neutral water molecules bonded by hydrogen bonds) in the material, drying and dehydrating at 300-550 ℃ for 0.5-1.5 h: (NH) 4 ) 2 V 6 O 16 ·nH 2 O→(NH 4 ) 2 V 6 O 16 +nH 2 O；
And a second stage: removing crystal water in the material, decomposing, reacting at 550-650 ℃ for 2.5-3.5 h with deamination and dehydration of bound water (water bound by chemical bonds): (NH) 4 ) 2 V 6 O 16 →3V 2 O 5 +H 2 O↑+2NH 3 ↑；
And a third stage: oxidizing and melting reaction, at 650-800 ℃, melting reaction: v 2 O 5 (s)→V 2 O 5 (l)。
The smelting is divided into three stages, so that the phenomenon that the molten vanadium pentoxide directly contacts with water to generate violent reaction to cause instability in the furnace is avoided.
The invention realizes that the vanadium-containing material is piled into the inclined triangular material pile leading to the discharge hole by improving the melting furnace, realizes the continuous production mode of single-time feeding single-stage smelting or continuous feeding and continuous discharging according to the production requirement.
In the continuous production smelting process, the temperature for oxidizing and melting vanadium is controlled to be 676-800 ℃, so that the upper-layer materials of the inclined triangular material piles are firstly melted and then left out through the discharge port, then the vanadium-containing material layers are supplemented to the two inclined triangular material piles through the feed port (1), one supplemented layer is melted, and the lower-layer materials which are not melted can realize the effect of melting and discharging, thereby realizing the continuous production mode of 'continuous feeding and continuous discharging'. Specifically, according to the invention, the oxidation melting temperature is controlled, the feeding speed is 0.5-1 t/h for each feeding port, and the total feeding speed of the two feeding ports is 1-2 t/h, so that the feeding amount is matched with the material melting outflow speed, and continuous feeding smelting is carried out.
In the charging process, the lower layer of the material pile is permeated by the heat of the melting material on the upper layer, the material pile is completely dehydrated and deaminated as early as possible without oxidation and melting, the upper layer of the material pile is a newly added material, the newly added material is very thin in thickness and can be quickly deaminated and dehydrated under the heat permeation action of the material on the lower layer, and the material pile can quickly enter a vanadium oxidation melting stage under the action of a heat source, so that the continuous melting after the continuous charging is kept. The charging time can be carried out at any time in the smelting process, for example, the continuous charging is started from the beginning of charging materials, and the continuous charging can also be started when the materials in the furnace begin to melt and flow out; but the continuity can be realized whenever the vanadium-containing material layer is supplemented to the two inclined triangular material piles.
In the single-stage production smelting process, all materials can be added at one time, and batch materials can also be added in the smelting process; in addition, the lower layer material which is not melted is permeated by heat in the melting process of the upper layer material, is completely dehydrated and deaminated as early as possible, does not need to be heated in the later stage of smelting, and can realize the effect of melting and discharging at constant temperature.
In the method, the vanadium-containing material is ammonium polyvanadate.
In the method, the method also comprises the following steps in order to obtain the finished flaky vanadium pentoxide product: E. and after the molten material is discharged from the discharge port (4), the sheet is cast by a sheet casting device to obtain the sheet vanadium pentoxide.
The invention also relates to a melting furnace which is matched with the method and comprises two feeding ports (1), two heat sources (2) and a discharging port (4); wherein, the feed inlet (1) is positioned at the top of the furnace, the two heat sources (2) are arranged oppositely, and the discharge outlet (4) is positioned at the bottom of the furnace.
The specification of the melting furnace can be designed according to actual needs, and the method and the melting furnace can realize continuous production, so the melting furnace can be provided withFor large scale furnaces to increase throughput, for example, in the present example the furnace floor area is designed to be F =20m 2 Production capacity 380kg V 2 O 5 /m 2 D; the method of the invention is matched with the improvement of the batch melting furnace, and can even exceed the designed capacity.
The present invention is further illustrated by the following examples, without thereby limiting the scope of the invention to the examples described.
Examples 1 and 2 use a melting furnace as described in figure 1 with a hearth area of F =20m 2 Production capacity 380kg V 2 O 5 /m 2 ·d。
Example 1: continuous smelting production
A. In the whole smelting process, continuously adding vanadium-containing materials into the melting furnace through the charging hole (1) at a charging speed of 1t/h (the charging speed of each charging hole is 0.5 t/h), and piling the vanadium-containing materials into two inclined triangular material piles (3) leading to the discharging hole (4);
B. the temperature in the furnace is controlled to 400 +/-50 ℃ through a heat source (2) to carry out drying and dehydration for 1h;
C. then controlling the temperature in the furnace to 600 +/-50 ℃, and performing deamination and dehydration for 3 hours;
D. finally, controlling the temperature in the furnace to reach 700 +/-50 ℃, carrying out vanadium oxidation and melting, wherein the molten material is immediately melted out from a discharge port (4), and meanwhile, continuously adding the vanadium-containing material through a feed port (1) in the step A, supplementing the material in the furnace, and realizing continuous production;
E. and after the molten material is discharged from the discharge port (4), the sheet is cast by a sheet casting device to obtain the sheet vanadium pentoxide.
Smelting phenomenon: the vanadium loss in the smoke is very little and invisible in the smelting process.
The yield of the flaky vanadium pentoxide is 0.63t/h, and the vanadium grade is V 2 O 5 =98.17% -98.96%, and the smelting yield is 99.35%.
Example 2: single stage smelting production
Adding vanadium-containing materials into the melting furnace through a feed inlet (1) (5 tons of APV are added into each feed inlet), and piling the vanadium-containing materials into two inclined triangular material piles (3) leading to a discharge outlet (4);
B. controlling the temperature in the furnace to 400 +/-50 ℃ by a heat source (2), and drying and dehydrating for 1h;
C. then controlling the temperature in the furnace to 600 +/-50 ℃, and carrying out deamination and dehydration for 3h;
D. finally, controlling the temperature in the furnace to 700 +/-50 ℃, carrying out vanadium oxidation and melting, and melting out the molten material from a discharge hole (4);
E. and after the molten material is discharged from the discharge port (4), the sheet is cast by a sheet casting device to obtain the sheet vanadium pentoxide.
Smelting phenomenon: the vanadium loss in the smoke is very little and invisible in the smelting process.
After the smelting is finished, the yield of the flaky vanadium pentoxide is 6.3 tons, and the vanadium grade is V 2 O 5 =98.19% and the smelting yield is 98.98%.
Comparative example 1
Adopting a 2112 material distribution mode, wherein the smelting temperature is as follows: the blank material is divided into three temperature sections: 1h smelting at 700-800 ℃ in the section I, 3h smelting at 800-850 ℃ in the section II, and 1h smelting at 850-900 ℃ in the section III; discharging: smelting for 3.5h at 900-1000 ℃.
Smelting phenomenon: the smoke in the furnace is heavy, the loss of vanadium in the smoke is large, and the smoke is clear and visible.
The smelting effect is as follows: adopting the prior process, intermittently smelting 16 furnaces, and adding APV (namely red vanadium and polyvanadate according to average water content H) in total 2 O =29.66%, vanadium grade TV = 49.57%) 93.54 ton, yielding 57.78 ton (vanadium grade V) of flaky vanadium pentoxide in total 2 O 5 = 97.68%), the smelting yield is only 96.91%; the average APV of the single furnace is about 5.86 tons, and the average discharge amount of the vanadium flakes is 3.62 tons.
Claims (5)
1. The method for smelting vanadium pentoxide by using the melting furnace is characterized by comprising the following steps: the method comprises the following steps:
A. adding vanadium-containing materials into the melting furnace through a feed inlet (1), and stacking the vanadium-containing materials into two inclined triangular material piles (3) leading to a discharge outlet (4);
B. controlling the temperature in the furnace to reach 300-550 ℃ through a heat source (2), and drying and dehydrating;
C. then controlling the temperature in the furnace to be 550 to 650 ℃, and carrying out deamination dehydration;
D. finally, controlling the temperature in the furnace to reach 676 to 800 ℃, carrying out vanadium oxidation and melting, and melting the molten material out from a discharge hole (4);
in the smelting process, a vanadium-containing material layer is supplemented to the two inclined triangular material piles through the feeding port (1), and a supplemented layer is melted.
2. The method for smelting vanadium pentoxide by using a melting furnace according to claim 1, wherein: the vanadium-containing material is ammonium polyvanadate.
3. The method for smelting vanadium pentoxide by use of the melting furnace according to claim 1, wherein: the drying and dehydrating time is 0.5 to 1.5h.
4. The method for smelting vanadium pentoxide by using a melting furnace according to claim 1, wherein: the time for deamination and dehydration is 2.5 to 3.5 hours.
5. The method for smelting vanadium pentoxide by using the melting furnace according to any one of claims 1 to 4, wherein:
E. and after the molten material is discharged from the discharge port (4), the sheet is cast by a sheet casting device to obtain the sheet vanadium pentoxide.
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| CN114149026B (en) * | 2021-11-15 | 2023-12-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium pentoxide by taking ammonium vanadate as raw material |
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