CN101289226A - Process for preparing vanadic anhydride by vacuum calcining ammonium poly-vanadate - Google Patents
Process for preparing vanadic anhydride by vacuum calcining ammonium poly-vanadate Download PDFInfo
- Publication number
- CN101289226A CN101289226A CNA200810058163XA CN200810058163A CN101289226A CN 101289226 A CN101289226 A CN 101289226A CN A200810058163X A CNA200810058163X A CN A200810058163XA CN 200810058163 A CN200810058163 A CN 200810058163A CN 101289226 A CN101289226 A CN 101289226A
- Authority
- CN
- China
- Prior art keywords
- vacuum
- vanadate
- vanadium pentoxide
- stove
- flakes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 56
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 24
- 238000001354 calcination Methods 0.000 title claims abstract description 17
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims description 21
- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 27
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000009615 deamination Effects 0.000 claims abstract description 9
- 238000006481 deamination reaction Methods 0.000 claims abstract description 9
- 238000005272 metallurgy Methods 0.000 claims abstract description 8
- 230000018044 dehydration Effects 0.000 claims abstract description 7
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 20
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000009835 boiling Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A method for preparing vanadium pentoxide by calcining ammonium polyvanadate in vacuum is disclosed. The invention relates to the method for preparing the vanadium pentoxide by utilizing the ammonium polyvanadate, which pertains to the technical field of metallurgy chemical. The method is characterized in that industrial ammonium polyvanadate is smashed and then put into a vacuum metallurgical furnace to be heated and calcined in vacuum to prepare the vanadium pentoxide; industrial pure oxygen with low pressure is led in the vacuum metallurgical furnace so as to ensure the oxidizing atmosphere in the furnace and the pressure in the furnace is controlled to be 0.2atm to 0.3atm. The invention has the advantages that the reaction is carried out in vacuum; the reaction temperature is lower compared with normal pressure, therefore, the energy consumption is lower; under the condition of vacuum, part of impurities with low boiling point can be removed by volatilization so that the content of the impurities in the product is reduced, thus ensuring the vanadium pentoxide to be high in purity; the whole processes of dehydration, deamination and melting can be completed simultaneously in the same reactor and the operation is simple and easy to control, metal recycle rate is high and production cost is low.
Description
Technical field
The present invention relates to a kind ofly produce the method for Vanadium Pentoxide in FLAKES, belong to the chemical metallurgy technical field with ammonium poly-vanadate.
Background technology
Ammonium poly-vanadate (APV) or ammonium meta-vanadate (NH
4VO
3) calcining deamination produce V
2O
5Be an important step in the vanadium metallurgical process, from ammonium poly-vanadate (APV) or ammonium meta-vanadate (NH
4VO
3) obtain piece of Vanadium and generally will pass through dehydration, deamination and three steps of fusing.Industrial fusing ammonium poly-vanadate film-making vanadium; external three sections method of fusion that adopt more; promptly at first in moisture eliminator controlled temperature dewater for 100~200 ℃; then in rotary kiln through 550 ℃ of left and right sides deaminations; obtain the powdery Vanadium Pentoxide in FLAKES; at last the powdery Vanadium Pentoxide in FLAKES is melted in 750 ℃ of left and right sides electric furnaces, come out of the stove after the rotation granulation platform of water-cooled is cast certain thickness thin slice, the rate of recovery of this method vanadium can reach more than 99%.China's fusing ammonium poly-vanadate film-making vanadium all adopts single stage method at present, promptly finishes dehydration, deamination and three steps of fusing at same seat smelting furnace.Smelting furnace adopts reverberatory furnace, has ring flange that it is divided into three zones in the stove: first zone is drying zone, and controlled temperature is 300~450 ℃; Second zone is the resolver, and controlled temperature is 450~600 ℃; The 3rd zone be melt oxidation district temperature greater than 650 ℃, the rate of recovery of this method vanadium is generally about 95%.
Though three sections external method of fusion vanadium recovery height exist that facility investment is big, complicated operation and production link is many, labour productivity is low defective.Domestic single stage method, not only vanadium recovery is on the low side, and temperature is wayward, if the too high meeting of temperature causes the volatilization loss of Vanadium Pentoxide in FLAKES in melting process, especially more than 900 ℃, the vanadium loss is serious, because drying and fusing are to carry out in a stove simultaneously, dried powdery Vanadium Pentoxide in FLAKES is easy to be blown away by hot blast, also can cause the loss of vanadium.The nitrogen that is decomposited by ammonium poly-vanadate at high temperature can decompose release hydrogen in addition, Vanadium Pentoxide in FLAKES is reduced to infusible barium oxide at a low price, have only and after ammonia is all deviate from, the low price vanadium could be continued to be oxidized to the low-melting Vanadium Pentoxide in FLAKES of high price, therefore single stage method not only the cycle long, heat utilization efficiency is low, energy consumption is high, and vanadium recovery is on the low side.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of vacuum calcining ammonium poly-vanadate is produced Vanadium Pentoxide in FLAKES, can finish dehydration, deamination and melting process simultaneously, and technology is simple and easy to control, easy to operate, energy-efficient, product purity is high.
Solving the scheme that technical problem of the present invention adopts is: carry out the heating under vacuum calcining with putting into the vacuum metallurgy stove after the fragmentation of industrial pie ammonium poly-vanadate, in vacuum oven, finish dehydration, deamination and three processes of fusing continuously, produce Vanadium Pentoxide in FLAKES, and feed pure oxygen in the vacuum oven, to guarantee oxidizing atmosphere in the stove.
A kind of vacuum calcining ammonium poly-vanadate is produced the method for Vanadium Pentoxide in FLAKES, it is characterized in that, carries out the heating under vacuum calcining with putting into the vacuum metallurgy stove after the fragmentation of industrial pie ammonium poly-vanadate, produces Vanadium Pentoxide in FLAKES.Feed the low-pressure industrial pure oxygen in the vacuum oven, with oxidizing atmosphere in the assurance stove, and the control furnace pressure is 0.05~0.3atm.
Concrete processing condition of the present invention are: (1) is crushed to the fritter of 0.5cm~1cm with ammonium poly-vanadate, and the acid-resistant stainless steel disk of packing into is sent into vacuum oven; (2) vacuum oven vacuumizes, and makes furnace pressure≤100Pa; In stove, feed industrial pure oxygen, make furnace pressure remain on 0.2atm~0.3atm; (3) regulate heating power, 350 ℃~450 ℃ of controlled temperature carry out vacuum-drying, calcining 90min~150min, and expellant gas imports the ammonia absorption unit in this process; (4) close the inlet mouth valve, stop logical oxygen in stove, continue to vacuumize, furnace pressure is remained on≤100Pa; (5) regulate heating power, 500 ℃~600 ℃ of controlled temperature carry out vacuum melting 10min~30min; (6) close heater switch, stop to vacuumize, 3min~5min is placed in the Vanadium Pentoxide in FLAKES continuation of molten state in vacuum oven, the water-cooled of coming out of the stove then casting sheet obtains piece of Vanadium.
Primitive reaction of the present invention is as follows:
(NH
4)
6V
10O
28·nH
2O→(NH
4)
6V
10O
28+nH
2O (1)
3(NH
4)
6V
10O
28→5(NH
4)
2V
6O
16+8NH
3+4H
2O (2)
2(NH
4)
2V
6O
16+3O
2→6V
2O
5+8H
2O+2N
2 (3)
Described ammonium poly-vanadate is moisture 30~40% industrial pie ten ammonium vanadate ((NH
4)
6V
10O
28).
The invention has the beneficial effects as follows:
Ammonium poly-vanadate of the present invention is produced the process of Vanadium Pentoxide in FLAKES and is carried out under vacuum condition, and temperature of reaction is than low under the normal pressure, and energy consumption is low; Under the vacuum condition, the part lower-boiling impurity is removed by volatilization simultaneously, be reduced the product foreign matter content, Vanadium Pentoxide in FLAKES product purity height.Can finish the whole process of dehydration, deamination and fusing in same reactor simultaneously, easy control simple to operate, metal recovery rate height, production cost are low.
Embodiment
Example one: raw material is moisture 32% industrial pie ten ammonium vanadate ((NH
4)
6V
10O
28NH
2O) 3.0kg is crushed to the fritter of 0.5~1cm, and the acid-resistant stainless steel disk of packing into is sent into the vacuum metallurgy stove; Vacuum oven vacuumizes, and makes furnace pressure≤100Pa, feeds industrial pure oxygen in stove, makes furnace pressure remain on 0.2atm, heat temperature raising; Regulate heating power, 400 ℃ of controlled temperature carry out vacuum-drying, calcining 90min.Expellant gas imports the ammonia absorption unit in this process; Close the inlet mouth valve, stop logical oxygen in stove, continue to vacuumize, furnace pressure is remained on≤100Pa; Regulate heating power, 550 ℃ of controlled temperature carry out vacuum melting 10min; Close heater switch, stop to vacuumize, 3min is placed in the Vanadium Pentoxide in FLAKES continuation of molten state in vacuum oven, the water-cooled of coming out of the stove then casting sheet obtains piece of Vanadium 1.76kg.
Product pentoxide content 98.9%, the rate of recovery 99.7% of vanadium.
Example two: raw material is moisture 35% industrial pie ten ammonium vanadate ((NH
4)
6V
10O
28NH
2O) 3.0kg is crushed to the fritter of 0.8cm, and the acid-resistant stainless steel disk of packing into is sent into the vacuum metallurgy stove; Vacuum oven vacuumizes, and makes furnace pressure≤100Pa, feeds industrial pure oxygen in stove, makes furnace pressure remain on 0.2atm, heat temperature raising; Regulate heating power, 450 ℃ of controlled temperature carry out vacuum-drying, calcining 120min.Expellant gas imports the ammonia absorption unit in this process; Close the inlet mouth valve, stop logical oxygen in stove, continue to vacuumize, furnace pressure is remained on≤100Pa; Regulate heating power, 580 ℃ of controlled temperature, vacuum melting 30min; Close heater switch, stop to vacuumize, 4min is placed in the Vanadium Pentoxide in FLAKES continuation of molten state in vacuum oven, the water-cooled of coming out of the stove then casting sheet obtains piece of Vanadium 1.67kg.
Product pentoxide content 99.2%, the rate of recovery 99.5% of vanadium.
Example three: raw material is moisture 37% industrial pie ten ammonium vanadate ((NH
4)
6V
10O
28NH
2O) 3.0kg is crushed to the fritter of 0.5cm, and the acid-resistant stainless steel disk of packing into is sent into the vacuum metallurgy stove; Vacuum oven vacuumizes, and makes furnace pressure≤100Pa, feeds industrial pure oxygen in stove, makes furnace pressure remain on 0.3atm, heat temperature raising; Regulate heating power, 380 ℃ of controlled temperature carry out vacuum-drying, calcining 120min.Expellant gas imports the ammonia absorption unit in this process; Close the inlet mouth valve, stop logical oxygen in stove, continue to vacuumize, furnace pressure is remained on≤100Pa; Regulate heating power, 600 ℃ of controlled temperature carry out vacuum melting 20min; Close heater switch, stop to vacuumize, 3min is placed in the Vanadium Pentoxide in FLAKES continuation of molten state in vacuum oven, the water-cooled of coming out of the stove then casting sheet obtains piece of Vanadium 1.62kg.
Product pentoxide content 99.5%, the rate of recovery 99.6% of vanadium.
Claims (3)
1. a vacuum calcining ammonium poly-vanadate is produced the method for Vanadium Pentoxide in FLAKES, it is characterized in that: carry out the heating under vacuum calcining putting into the vacuum metallurgy stove after the fragmentation of industrial pie ammonium poly-vanadate, in vacuum oven, finish dehydration, deamination and three processes of fusing continuously, produce Vanadium Pentoxide in FLAKES, and feed pure oxygen in the vacuum oven, to guarantee oxidizing atmosphere in the stove.
2. vacuum calcining ammonium poly-vanadate according to claim 1 is produced the method for Vanadium Pentoxide in FLAKES, it is characterized in that: (1) is crushed to the fritter of 0.5cm~1cm with ammonium poly-vanadate, and the acid-resistant stainless steel disk of packing into is sent into vacuum oven; (2) vacuum oven vacuumizes, and makes furnace pressure≤100Pa; In stove, feed industrial pure oxygen, make furnace pressure remain on 0.2atm~0.3atm; (3) regulate heating power, 350 ℃~450 ℃ of controlled temperature carry out vacuum-drying, calcining 90min~150min, and expellant gas imports the ammonia absorption unit in this process; (4) close the inlet mouth valve, stop logical oxygen in stove, continue to vacuumize, furnace pressure is remained on≤100Pa; (5) regulate heating power, 500 ℃~600 ℃ of controlled temperature carry out vacuum melting 10min~30min; (6) close heater switch, stop to vacuumize, 3min~5min is placed in the Vanadium Pentoxide in FLAKES continuation of molten state in vacuum oven, the water-cooled of coming out of the stove then casting sheet obtains piece of Vanadium.
3. vacuum calcining ammonium poly-vanadate according to claim 1 is produced the method for Vanadium Pentoxide in FLAKES, it is characterized in that: described ammonium poly-vanadate is the industrial pie ten ammonium vanadate (NH that water content accounts for gross weight 30~40%
4)
6V
10O
28
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CN200810058163XA CN101289226B (en) | 2008-03-07 | 2008-03-07 | Process for preparing vanadic anhydride by vacuum calcining ammonium poly-vanadate |
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CN101289226A true CN101289226A (en) | 2008-10-22 |
CN101289226B CN101289226B (en) | 2010-07-21 |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102502829A (en) * | 2011-11-18 | 2012-06-20 | 吉首大学 | Production process for preparing high-purity vanadium pentoxide by means of calcining and decomposing metavanadic acid |
CN102616848A (en) * | 2012-02-27 | 2012-08-01 | 河北钢铁股份有限公司承德分公司 | Production method and production system for vanadium pentoxide |
CN103922403A (en) * | 2014-03-24 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing powdery vanadic anhydride by ammonium polyorthovanadate in fluidization state |
CN108358242A (en) * | 2018-04-17 | 2018-08-03 | 中国科学院过程工程研究所 | A kind of nitrogen element content is less than the preparation method of the vanadic anhydride of ten a ten thousandths |
CN108358241A (en) * | 2018-04-17 | 2018-08-03 | 中国科学院过程工程研究所 | A kind of carbon element content is less than the preparation method of the vanadic anhydride of a ten thousandth |
CN108358243A (en) * | 2018-04-17 | 2018-08-03 | 中国科学院过程工程研究所 | A kind of preparation method of vanadic anhydride of the tetravalence content of vanadium less than 5/100000ths |
CN109319839A (en) * | 2018-11-28 | 2019-02-12 | 湖南众鑫新材料科技股份有限公司 | A kind of high-purity lamellar vanadic anhydride and preparation method thereof |
CN114180625A (en) * | 2021-11-15 | 2022-03-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying vanadium pentoxide by negative pressure volatilization |
-
2008
- 2008-03-07 CN CN200810058163XA patent/CN101289226B/en not_active Expired - Fee Related
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102502829A (en) * | 2011-11-18 | 2012-06-20 | 吉首大学 | Production process for preparing high-purity vanadium pentoxide by means of calcining and decomposing metavanadic acid |
CN102616848A (en) * | 2012-02-27 | 2012-08-01 | 河北钢铁股份有限公司承德分公司 | Production method and production system for vanadium pentoxide |
CN103922403A (en) * | 2014-03-24 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing powdery vanadic anhydride by ammonium polyorthovanadate in fluidization state |
CN103922403B (en) * | 2014-03-24 | 2015-09-16 | 攀钢集团攀枝花钢铁研究院有限公司 | The method of powdery Vanadium Pentoxide in FLAKES is produced in a kind of ammonium poly-vanadate fluidization |
CN108358242A (en) * | 2018-04-17 | 2018-08-03 | 中国科学院过程工程研究所 | A kind of nitrogen element content is less than the preparation method of the vanadic anhydride of ten a ten thousandths |
CN108358241A (en) * | 2018-04-17 | 2018-08-03 | 中国科学院过程工程研究所 | A kind of carbon element content is less than the preparation method of the vanadic anhydride of a ten thousandth |
CN108358243A (en) * | 2018-04-17 | 2018-08-03 | 中国科学院过程工程研究所 | A kind of preparation method of vanadic anhydride of the tetravalence content of vanadium less than 5/100000ths |
CN109319839A (en) * | 2018-11-28 | 2019-02-12 | 湖南众鑫新材料科技股份有限公司 | A kind of high-purity lamellar vanadic anhydride and preparation method thereof |
CN109319839B (en) * | 2018-11-28 | 2021-03-23 | 湖南众鑫新材料科技股份有限公司 | High-purity flaky vanadium pentoxide and preparation method thereof |
CN114180625A (en) * | 2021-11-15 | 2022-03-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying vanadium pentoxide by negative pressure volatilization |
CN114180625B (en) * | 2021-11-15 | 2023-11-07 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying vanadium pentoxide by negative pressure volatilization |
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