CN101717117A - Method for producing vanadium trioxide - Google Patents
Method for producing vanadium trioxide Download PDFInfo
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- CN101717117A CN101717117A CN200910312502A CN200910312502A CN101717117A CN 101717117 A CN101717117 A CN 101717117A CN 200910312502 A CN200910312502 A CN 200910312502A CN 200910312502 A CN200910312502 A CN 200910312502A CN 101717117 A CN101717117 A CN 101717117A
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- Prior art keywords
- vanadium
- vanadous oxide
- raw material
- production method
- gas
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 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 abstract 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 30
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 230000009467 reduction Effects 0.000 claims abstract description 25
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 25
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 238000005453 pelletization Methods 0.000 claims description 47
- 239000007789 gas Substances 0.000 claims description 27
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 21
- 239000000428 dust Substances 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 229920001353 Dextrin Polymers 0.000 claims description 10
- 239000004375 Dextrin Substances 0.000 claims description 10
- 235000019425 dextrin Nutrition 0.000 claims description 10
- 229920002472 Starch Polymers 0.000 claims description 8
- 235000019698 starch Nutrition 0.000 claims description 8
- 239000008107 starch Substances 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000003034 coal gas Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 abstract description 30
- 238000000034 method Methods 0.000 abstract description 21
- 238000011084 recovery Methods 0.000 abstract description 20
- 239000007787 solid Substances 0.000 abstract description 10
- 230000036632 reaction speed Effects 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000008188 pellet Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 230000002829 reductive effect Effects 0.000 description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 18
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005243 fluidization Methods 0.000 description 4
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 4
- 238000011946 reduction process Methods 0.000 description 4
- 238000001149 thermolysis Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- 229910001199 N alloy Inorganic materials 0.000 description 1
- 229910000756 V alloy Inorganic materials 0.000 description 1
- LOUBVQKDBZRZNQ-UHFFFAOYSA-M [O-2].[O-2].[OH-].O.[V+5] Chemical compound [O-2].[O-2].[OH-].O.[V+5] LOUBVQKDBZRZNQ-UHFFFAOYSA-M 0.000 description 1
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the chemical field, in particular to a method for producing vanadium trioxide, aiming at improving the reaction speed of the method for producing vanadium trioxide and providing a solution as follows: A. raw material preparation; B. reduction of the prepared raw material by using reducing gas; and C. obtaining vanadium trioxide after reduction. The improvement of the method in the invention is that the used raw material in step A is composed of binder, carbon powder and vanadium-containing material, wherein the vanadium-containing material is ammonium vanadate or vanadium pentoxide. The invention adopts the technologies of carbon-proportioning and pellet preparation aiming at the raw material to enable the raw material to react in a gas-solid bi-phase reducing agent formed by solid carbon powder and reducing gas, thus improving the reduction reaction speed, enhancing recovery rate of the vanadium, and reducing consumption of the reducing gas. The produced pellet has the advantages of improving reaction speed, avoiding and reducing volatilization of vanadium-containing powder material, protecting environment and being beneficial for labor protection.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of method of producing vanadous oxide.
Background technology
Vanadous oxide is the reductive agent of smelting ferrovanadium alloy or other vanadium alloy, as VN alloy and high vanadium ferroalloy.Can reduce during with its smelting ferrovanadium and produce this, improve vanadium recovery.Can improve speed of response with its preparation VN alloy, improve the vanadium-nitrogen alloy product quality.The preparation method of vanadous oxide roughly can reduce two kinds: a kind of is the ammonium vanadate thermolysis cracking process of not additional reducing agent; Another kind is the direct-reduction process of additional reducing agent.Main preparation method is as follows:
(a) the ammonium vanadate thermolysis cracking process of additional reducing agent not
Japanese patent application 72/7447294 discloses with ammonium meta-vanadate and has been heated in hydrogen under 200～400 ℃ of conditions, and vanadous oxide is produced in reduction in the silica tube container, and its shortcoming is a reduction apparatus manufacturing cost height.
The U.S.: U.S. combinating carbide company has obtained to produce the patent of vanadous oxide in the U.S. in nineteen sixty-eight.As raw material, under the condition that does not add any reductive agent, the nescent hydrogen that the thermo-cracking by the ammonia that discharges of heating ammonium meta-vanadate produces reduces ammonium meta-vanadate to this inventive method with ammonium meta-vanadate, thereby but continuous high-efficient is produced the vanadous oxide of based on very high purity.
France: Union Carbide Corporation also is to utilize ammonium vanadate to produce vanadous oxide in the patent that France obtains, and its technological process is, at water vapour, NH
3And NH
3Thermolysis produces under the condition of hydrogen, with NH
4VO
3Or NH
4VO
3Thermal decomposition product, for example (NH
4)
2V
6O
16(NH
4)
2O2V
2O
45V
2O
5(NH
4) 6V
16O
28Pure V is produced in reduction continuously
2O
3
(b) the direct reductive agent method of additional reducing agent
Japanese Patent 86/141, the 622 disclosed technical schemes of producing vanadous oxide: with the Vanadium Pentoxide in FLAKES is raw material, with ammonia as reductive agent, the thermal decomposition and reduction process is carried out under the stainless steel tube mesohigh, the shortcoming that this technical scheme exists is, recovery time reaches 4 hours, makes high pressure resistant reduction vessel cost height.
Japanese patent application 88/01320228 discloses a kind of technical scheme of producing vanadous oxide: is raw material with granularity for-150 purpose ammonium meta-vanadates, is reductive agent with hydrogen, with its thermolysis and be reduced to vanadous oxide.The shortcoming of this technical scheme is: the recovery time reaches 10-20 hour.
Japanese patent application 84/61141622 discloses with the high price barium oxide under ammonia atmosphere, is pressed under the 450--650 ℃ of condition at the 0.1-1.5 atmosphere, reduces 1-6 hour, produce vanadous oxide, the shortcoming of its method is: High Temperature High Pressure, long reaction time, reduction apparatus cost height.
U.S. Patent Publication produce the production technique of vanadous oxide with Vanadium Pentoxide in FLAKES, its method is the barium oxide particle mixture (V based on Vanadium Pentoxide in FLAKES of packing in fluidized-bed reactor
2O
5Account for more than 98%), feeding under the hydrogen condition, reduce about heating barium oxide to 593 ℃, time is a few hours, solid particulate after reduction mainly is made up of vanadous oxide, but the degree that some particle is reduced is less, thereby forms vanadium tetraoxide.In addition, some particle is that shell is reduced, thereby granule interior still is a Vanadium Pentoxide in FLAKES.In general, those partial reductions particle, its vanadiumcontent is 65%～68%, is the particle of pure vanadous oxide basically as for those, vanadiumcontent then is 68%.
Russia produces V
2O
3Raw material almost all adopt Vanadium Pentoxide in FLAKES.Reductive agent has NH
3With vanadium metal etc.People such as Yankelevich have announced that in 1974 they use NH
3Reduction V
2O
5Produce V
2O
3Method.This technology top condition is: 450 ℃ of temperature, NH
3Flow 4L/h, recovery time 3h.Obtained to produce the USSR (Union of Soviet Socialist Republics) patent of vanadous oxide in 1976 with Vanadium Pentoxide in FLAKES people such as the inorganic and worker Yankelevich of general chemistry institute of USSR (Union of Soviet Socialist Republics) academy of sciences.Employed reductive agent is NH in the patent gazette
3, Heating temperature is still selected 450 ℃.
To sum up, the existing vanadous oxide production technique of producing has following shortcoming: long reaction time, reduction temperature height, complex manufacturing, High Temperature High Pressure and the rate of recovery are low etc.Desire of the present invention realizes improving speed of response, simplifies production technique, improves vanadous oxide purity, reduces purposes such as gas consumption and saving cost by the improvement prior art.
Summary of the invention
The present invention provides following solution in order to improve the speed of response of vanadous oxide production method:
The production method of vanadous oxide comprises the steps:
A, preparation raw material;
B, the raw material of preparation is adopted the reducing gas reduction;
C, reduction promptly get vanadous oxide.
The improvements of the inventive method be the described raw material of steps A by binding agent, carbon dust, contain the vanadium material and form; The wherein said vanadium material that contains is ammonium vanadate or Vanadium Pentoxide in FLAKES.It with magnitude relation is: the binding agent add-on is the 0.5%-2% that contains the vanadium weight of material, and the carbon dust add-on is the 0.5-3% that contains the vanadium weight of material.
Above-mentioned raw materials is mixed, make behind the pelletizing and the reducing gas reaction, the vanadous oxide that reaction conditions can adopt conventional temperature, time, reduction to obtain also adopts secluding air commonly used or protection of inert gas cooling process, finally obtains the vanadous oxide product.
The inventive method adopts the technology of joining carbon and preparation pelletizing at raw material, makes raw material mix in the reductive agent in the gas-solid two-phase of solid carbon dust and reducing gas composition and reacts, and has improved reduction reaction speed.The beneficial effect of the inventive method is as follows:
1, the solid carbon dust is formed gas-solid two-phase with reducing gas and is mixed reductive agent, has both improved reduction reaction speed, has reduced the consumption of reducing gas again.
2, adopt the pelletizing reduction technique, increased gas-solid two-phase reduction reaction specific surface area, realized rapid reaction.
3, pelletizing technology can reduce and contains vanadium powder dirt volatilization, both can improve the rate of recovery of vanadium, makes the rate of recovery can reach 99.7%; Can reduce environmental pollution again, and help labour protection.
4, obtain vanadous oxide with the inventive method and be used for producing products such as height, vanadium iron and VN alloy, belong to high quality raw material.Produce the rate of recovery high, that middle vanadium iron can improve vanadium.The production VN alloy had both improved the resultant velocity of VN alloy, can improve the quality of products again.
Embodiment
Below by specific description of embodiments of the present invention the explanation but do not limit the present invention.
The production method of vanadous oxide of the present invention comprises the steps:
A, preparation raw material;
B, the raw material of preparation is adopted the reducing gas reduction;
C, reduction promptly get vanadous oxide;
It is characterized in that: the described raw material of steps A is by binding agent, carbon dust, contains the vanadium material with ammonium vanadate or Vanadium Pentoxide in FLAKES etc. and forms.Its weight proportion is: the binding agent add-on is the 0.5%-2% of ammonium vanadate or Vanadium Pentoxide in FLAKES weight, and the carbon dust add-on is the 0.5-3% of ammonium vanadate or Vanadium Pentoxide in FLAKES weight.
During application, need raw material is mixed, make pelletizing after, react with reducing gas again.Raw material reacts in the gas-solid two-phase mixing reductive agent of solid carbon dust and reducing gas composition, has improved reduction reaction speed, can also improve the rate of recovery of vanadium, reduces reducing gas consumption.Make pelletizing and not only can improve speed of response, can also avoid reducing the volatilization that contains vanadium powder shape material, both protected environment, help labour protection again.
Further, control pelletizing granularity is 4-8mm, and granularity is if exceed this scope, and pelletizing reduction reaction speed slows down.
If pelletizing is moist, and easily fragmentation influences reduction effect in reduction process, so and should be dry earlier before the reducing gas reaction.After the pelletizing drying, pellet strength increases, and guarantees that in reduction process pelletizing is not broken.Be to guarantee drying efficiency, drying temperature＞100 ℃ more than time of drying＞4h, by above-mentioned forced drying condition, can guarantee pellet strength.
In the inventive method, binding agent is one or more of dextrin, starch, wilkinite, water glass, magnesium chloride or water; Carbon dust is industrial carbon dust or Graphite Powder 99.
In step B when reduction,, the reducing gas that adopts was one or more of blast furnace gas, coke-oven gas, coal gas of converter, electric furnace coal gas, producer gas, hydrogen, ammonia.Can consider according to cost and security aspect during concrete the application, select suitable gas.
Further, the reduction temperature condition is 500-650 ℃.Reduction reaction can be carried out at rotary kiln, fluidizing furnace, fluidized bed furnace, shaft furnace or pushed bat kiln.Reduction reaction probably carries out can obtaining vanadous oxide in 10-30 minute.
After reduction obtained vanadous oxide, under the condition of secluding air or protection of inert gas, be cooled to 100 ℃ and come out of the stove.
Embodiment 1
Ammonium poly-vanadate powder, carbon dust and dextrin are mixed in mixing machine (the dextrin add-on is 2% of an ammonium poly-vanadate weight, the carbon dust add-on be ammonium poly-vanadate weight 1.5%), make ball then.The size-grade distribution of pelletizing is between 4～8 millimeters.The green-ball drying conditions is: 120～140 ℃ of drying temperatures; Time of drying＞6h.Carbon containing ammonium poly-vanadate pelletizing is joined in the external-heating rotary kiln continuously, with industrial gas and the reverse feeding rotary kiln of pelletizing direction of motion.Make by outer heating that the high-temperature zone reaches 500～650 ℃ in the rotary kiln, in the high-temperature zone insulation and keep about 15 minutes of recovery time, pelletizing decomposes and also is reduced to vanadous oxide.The vanadous oxide pelletizing is cooled to come out of the stove below 100 ℃ under argon shield, obtains the vanadous oxide pelletizing.
Vanadous oxide pelletizing ∑ V=67.86%, the rate of recovery 99.7% of vanadium.
Embodiment 2
Ammonium poly-vanadate powder, Graphite Powder 99, dextrin and starch are mixed in mixing machine (dextrin and starch add-on are respectively 1% of ammonium poly-vanadate weight, the Graphite Powder 99 add-on be ammonium poly-vanadate weight 1.5%), make ball then.The size-grade distribution of pelletizing is between 4～8 millimeters.The green-ball drying conditions is: 120～140 ℃ of drying temperatures; Time of drying＞6h.Carbon containing ammonium poly-vanadate pelletizing is joined in the fluidization boiler tube continuously from fluidization boiler tube middle and upper part, feed industrial gas from fluidization boiler tube bottom.Make by outer heating that the high-temperature zone reaches 500～650 ℃ in the fluidization boiler tube, in the high-temperature zone insulation and keep about 10 minutes of recovery time, pelletizing decomposes and also is reduced to vanadous oxide.The vanadous oxide pelletizing is cooled to come out of the stove below 100 ℃ under argon shield, obtains the vanadous oxide pelletizing.
Vanadous oxide pelletizing ∑ V=67.59%, the rate of recovery 99.5% of vanadium.
Embodiment 3
Ammonium poly-vanadate powder, Graphite Powder 99, dextrin and starch are mixed in mixing machine (dextrin and starch add-on are respectively ammonium poly-vanadate weight 1%, the Graphite Powder 99 add-on be ammonium poly-vanadate weight 1.5%), make ball then.The size-grade distribution of pelletizing is between 4～8 millimeters.The green-ball drying conditions is: 120～140 ℃ of drying temperatures; Time of drying＞6h.Carbon containing ammonium poly-vanadate pelletizing is joined in the shaft furnace continuously from shaft furnace top, feed industrial gas from the shaft furnace bottom.Make by induction heating that the high-temperature zone reaches 500～650 ℃ in the shaft furnace, in the high-temperature zone insulation and keep about 30 minutes of recovery time, pelletizing decomposes and also is reduced to vanadous oxide.The vanadous oxide pelletizing is cooled to come out of the stove below 100 ℃ under argon shield, obtains the vanadous oxide pelletizing.
Vanadous oxide pelletizing ∑ V=67.70%, the rate of recovery 99.6% of vanadium.
Embodiment 4
Vanadium Pentoxide in FLAKES powder, Graphite Powder 99, dextrin and starch are mixed in mixing machine (dextrin and starch add-on are respectively 1% of Vanadium Pentoxide in FLAKES weight, the Graphite Powder 99 add-on be Vanadium Pentoxide in FLAKES weight 1.5%), make ball then.The size-grade distribution of pelletizing is between 4～8 millimeters.The green-ball drying conditions is: 120～140 ℃ of drying temperatures; Time of drying＞6h.Carbon containing ammonium poly-vanadate pelletizing is joined in the shaft furnace continuously from shaft furnace top, feed Sweet natural gas from the shaft furnace bottom.Make by outer heating that the high-temperature zone reaches 500～650 ℃ in the shaft furnace, in the high-temperature zone insulation and keep about 25 minutes of recovery time, pelletizing decomposes and also is reduced to vanadous oxide.The vanadous oxide pelletizing is cooled to come out of the stove below 100 ℃ under argon shield, obtains the vanadous oxide pelletizing.
Vanadous oxide pelletizing ∑ V=67.73%, the rate of recovery 99.7% of vanadium.
Embodiment 5
Ammonium poly-vanadate powder, carbon dust and wilkinite are mixed (the wilkinite add-on is 1% of an ammonium poly-vanadate weight, and the carbon dust add-on is an ammonium poly-vanadate weight 1.5%) in mixing machine, make ball then.The size-grade distribution of pelletizing is between 4～8 millimeters.The green-ball drying conditions is: 120～140 ℃ of drying temperatures; Time of drying＞6h.Carbon containing ammonium poly-vanadate pelletizing is joined in the external-heating rotary kiln continuously, with industrial gas and the reverse feeding rotary kiln of pelletizing direction of motion.Make by outer heating that the high-temperature zone reaches 500～650 ℃ in the rotary kiln, in the high-temperature zone insulation and keep about 20 minutes of recovery time, pelletizing decomposes and also is reduced to vanadous oxide.The vanadous oxide pelletizing is cooled to come out of the stove below 100 ℃ under argon shield, obtains the vanadous oxide pelletizing.
Vanadous oxide pelletizing ∑ V=67.62%, the rate of recovery 99.6% of vanadium.
∑ V represents the quality percentage composition of full vanadium in the vanadous oxide pelletizing in the foregoing description.
To sum up, the inventive method compared with prior art reduction rate is faster, and is more efficient, and cost is lower, and environment is more friendly.
Claims (10)
1. the production method of vanadous oxide comprises the steps:
A, preparation raw material;
B, the raw material of preparation is adopted the reducing gas reduction;
C, reduction promptly get vanadous oxide;
It is characterized in that: the described raw material of steps A by binding agent, carbon dust, contain the vanadium material and form; The wherein said vanadium material that contains is ammonium vanadate or Vanadium Pentoxide in FLAKES.
2. the production method of vanadous oxide according to claim 1, it is characterized in that: raw material with magnitude relation is in the steps A: the binding agent add-on is the 0.5%-2% that contains the vanadium weight of material, and the carbon dust add-on is the 0.5-3% that contains the vanadium weight of material.
3. the production method of vanadous oxide according to claim 1 and 2 is characterized in that: the described raw material of steps A is mixed, make pelletizing after, react with reducing gas again.
4. the production method of vanadous oxide according to claim 3 is characterized in that: react with reducing gas after the described pelletizing drying again.
5. the production method of vanadous oxide according to claim 3, it is characterized in that: described pelletizing granularity is 4-8mm.
6. according to the production method of each described vanadous oxide of claim 1-5, it is characterized in that: described binding agent is one or more of dextrin, starch, wilkinite, water glass, magnesium chloride or water.
7. according to the production method of each described vanadous oxide of claim 1-5, it is characterized in that: described carbon dust is industrial carbon dust or Graphite Powder 99.
8. according to the production method of each described vanadous oxide of claim 1-5, it is characterized in that: described reducing gas is one or more of blast furnace gas, coke-oven gas, coal gas of converter, electric furnace coal gas, producer gas, hydrogen, ammonia.
9. according to the production method of each described vanadous oxide of claim 1-5, it is characterized in that: described reduction temperature condition is 500-650 ℃.
10. according to the production method of each described vanadous oxide of claim 1-5, it is characterized in that: after step C reduction obtains vanadous oxide, under the condition of secluding air or protection of inert gas, be cooled to 100 ℃ and come out of the stove.
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| CN2009103125027A CN101717117B (en) | 2009-12-29 | 2009-12-29 | Method for producing vanadium trioxide |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050491A (en) * | 2010-11-29 | 2011-05-11 | 中信锦州金属股份有限公司 | Vanadium trioxide production method |
| CN102583537A (en) * | 2012-02-27 | 2012-07-18 | 南通汉瑞实业有限公司 | Production process of vanadium trioxide |
| CN103359790A (en) * | 2012-03-31 | 2013-10-23 | 中国科学院合肥物质科学研究院 | Preparation method of vanadium trioxide or doped vanadium trioxide nano powder |
| CN103633309A (en) * | 2013-12-13 | 2014-03-12 | 黑龙江大学 | Preparation method of core-shell structure vanadium trioxide microspheres |
| CN103663555A (en) * | 2012-09-19 | 2014-03-26 | 大连博融新材料有限公司 | Granular vanadium oxide and production method thereof |
| CN103922404A (en) * | 2014-04-30 | 2014-07-16 | 攀枝花学院 | Method for preparing vanadium trioxide from vanadium pentoxide |
| CN104118910A (en) * | 2014-06-24 | 2014-10-29 | 中国科学院过程工程研究所 | Method for selectively preparing vanadium oxides and recovering hydroxides through vanadate hydrogen reduction method |
| CN104495926A (en) * | 2015-01-05 | 2015-04-08 | 南通汉瑞新材料科技有限公司 | Vanadium trioxide and preparation method thereof |
| CN105018970A (en) * | 2014-04-24 | 2015-11-04 | 东北大学 | Method for preparing vanadium metal through thermoelectric reduction in molten fluoride system |
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