CN101811734A - Method for producing vanadium pentoxide by microwave calcinations of ammonium metavanadate - Google Patents
Method for producing vanadium pentoxide by microwave calcinations of ammonium metavanadate Download PDFInfo
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- CN101811734A CN101811734A CN201010128309.0A CN201010128309A CN101811734A CN 101811734 A CN101811734 A CN 101811734A CN 201010128309 A CN201010128309 A CN 201010128309A CN 101811734 A CN101811734 A CN 101811734A
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- China
- Prior art keywords
- microwave
- vanadium pentoxide
- flakes
- temperature
- vanadate
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 78
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 title claims abstract description 27
- 238000001354 calcination Methods 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 20
- 235000019580 granularity Nutrition 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 description 8
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for producing vanadium pentoxide by microwave calcinations of ammonium metavanadate. The ammonium metavanadate and vanadium pentoxide powder are packed in a microwave reactor after drying respectively, wherein the weight of the vanadium pentoxide is 10 to 50 percent of the total weight; the microwave frequency is 2.45GHz; the power is 0 to 80kW; the calcining temperature is between 50 and 550DEG C; the time is 5 to 30 minutes; and the purity of the calcined products is 98.5 weight percent.
Description
One, technical field
The present invention relates to the method for a kind of serialization, mass-producing calcining production Vanadium Pentoxide in FLAKES, belong to vanadium metallurgical and material preparation technology and field of microwave heating.
Two, background technology
Vanadium Pentoxide in FLAKES is a kind of conventional ion absorption base material, moisture sensor, microbattery, electrochromic new function material of can be used as, also be a kind of catalyzer that is widely used in sulfuric acid industry, or the inhibiter of equipment anticorrosion in the decarburization in the ammonia synthesizing industry, sweetening agent and the petrochemical industry.According to relevant department prediction, the coming years, China will become in the world the vanadium produce market of tool potentiality, only satisfy one of the vanadium product that Iron and Steel Production consumes, and China is annual to need volume increase 30%.The supply demand gap of expectation to 2009 year China's vanadium product will reach more than 20,000 ton.
Vanadium mainly extracts from vanadium slag, bone coal and vanadium spent catalyst, and China mainly adopts the molten ammonium salt of sodium-salt calcination one water logging one Acid precipitation, one alkali to precipitate an ammonium meta-vanadate pyrolytic process.At present, the vanadium throw out mainly adopts conventional reverberatory furnace calcining, device structure is simple, easy to operate though this production method has, the advantage of easy control, has also that fuel consumption is big, thermo-efficiency is low (generally at 15-30%), the production cycle is long, cost is high, the purity of product and granularity be difficult to guarantee.In the technique for producing vanadium pentoxide that provides as patent CN101456587, ammonium meta-vanadate is to need calcining just can obtain Vanadium Pentoxide in FLAKES in 2 hours under 550 ℃ of conditions in temperature.
Three, summary of the invention
1. goal of the invention: microwave can add thermal material by the waste of energy selectivity in material inside as a kind of heating means of green high-efficient, has the incomparable advantages of conventional type of heating such as homogeneous heating, thermo-efficiency height, cleanliness without any pollution.The calcining that microwave is used for ammonium meta-vanadate has great importance for the raising that promotes Vanadium Pentoxide in FLAKES throughput and state of the art.The present invention is directed to the long deficiency of production cycle that aforesaid method exists, the method for the producing vanadium pentoxide by microwave calcinations of ammonium metavanadate of a kind of serialization, mass-producing is provided.
2. invention technical scheme: concrete grammar is realized by following steps:
(1) getting the raw materials ready, is the Vanadium Pentoxide in FLAKES product powder drying for standby respectively that 55 ℃ of granularities that will obtain through precipitation ammonium meta-vanadate that is 10-120 μ m and granularity are 10-100 μ m in temperature; Ammonium meta-vanadate that obtains and Vanadium Pentoxide in FLAKES are respectively charged into microwave device separately in the feed bin, regulate the feeding unit switch, the vanadium pentoxide powder that accounts for gross weight 10-50% is evenly allocated in the ammonium meta-vanadate powder, regulating the feed auger rotating speed is 3-10 rev/min, and material is delivered in the microwave device burner hearth continuously by feed auger;
(2) microwave calcination, microwave reactor frequency 2.45GHz, output rating is 0-80kW, the microwave device burner hearth is a microwave dedicated ceramic pipe, is with two to add feed bin; Regulate microwave output power, with 20-100 ℃/min temperature rise rate mixture being warming up to temperature is 500-550 ℃, and the control residence time of material in burner hearth is 5-30min;
(3) product discharging, temperature of charge to be mixed are opened drawing mechanism after rising to the preset temperature insulation, adjust the discharging of materials device rotating speed 2-10 commentaries on classics/clock, obtain the Vanadium Pentoxide in FLAKES product, and purity is 98.5wt/%; The Vanadium Pentoxide in FLAKES quality product V among the GB3283-87 that is up to state standards
2O
5-98 trade mark standards.
Design of the present invention is the weak ripple material of inhaling of ammonium meta-vanadate system, the temperature rise rate of ammonium meta-vanadate in microwave field is slow and can't reach its decomposition temperature, and the degradation production Vanadium Pentoxide in FLAKES of ammonium meta-vanadate belongs to the strong ripple material of inhaling, and can be heated to very high temperature at short notice.According to equivalent medium theory,, its temperature rise rate is accelerated and calcining and decomposing by in ammonium meta-vanadate, adding a certain proportion of Vanadium Pentoxide in FLAKES; Again calcination product is not produced any influence.In addition, in view of the Vanadium Pentoxide in FLAKES absorbing property is stronger, the present invention adopts the special preferably microwave dedicated ceramic of wave penetrate capability pipe to make burner hearth.The reaction formula that calcinations of ammonium metavanadate is produced Vanadium Pentoxide in FLAKES is:
2NH
4VO
3→V
2O
5+2NH
3+H
2O
(3) Fa Ming positively effect:
(1) present method equipment used adopts unique extra quality storehouse, simple helix feeding structure, has both guaranteed the material uniform mixing, has saved the Preblend operation again; (2) utilize the strong microwave absorbing property of Vanadium Pentoxide in FLAKES, the boosting calcinations of ammonium metavanadate can make its temperature rise rate accelerate and calcining and decomposing; Again calcination product is not produced any influence; (3) method is with short production cycle, has realized serialization, mass-producing operation, is suitable for suitability for industrialized production.
Four, embodiment:
Embodiment 1: with granularity is that 10-120 μ m ammonium meta-vanadate powder and granularity are that 10-100 μ m vanadium pentoxide powder places microwave device feed bin separately respectively after temperature is 55 ℃ of dryings, open the feeding unit switch, the by-pass cock aperture, the Vanadium Pentoxide in FLAKES that accounts for gross weight 10% is allocated in the ammonium meta-vanadate, regulating the feed auger rotating speed is 3 rev/mins, and mixture is delivered in the microwave device burner hearth; Open the microwave heating switch, regulate microwave output power to 10-15kW, with 20 ℃/min temperature rise rate mixture being warming up to temperature is 500-515 ℃; Open the drawing mechanism switch, adjusting the materials device rotating speed is 2 rev/mins, and the control residence time of material in burner hearth is 20min, and calcinate reclaims through discharge system and obtains the Vanadium Pentoxide in FLAKES product.Test by analysis, the Vanadium Pentoxide in FLAKES product purity reaches 98.7wt%, meets the V among the standard GB 3283-87
2O
5-98 trade mark standards.
Embodiment 2: with granularity is that 10-120 μ m ammonium meta-vanadate powder and granularity are that 10-100 μ m vanadium pentoxide powder places microwave device feed bin separately respectively after temperature is 55 ℃ of dryings, open the feeding unit switch, the by-pass cock aperture, the Vanadium Pentoxide in FLAKES that accounts for gross weight 25% is allocated in the ammonium meta-vanadate, regulating the feed auger rotating speed is 6 rev/mins, and mixture is delivered in the microwave device burner hearth; Open the microwave heating switch, regulate microwave output power to 40-45kW, with 50 ℃/min temperature rise rate mixture being warming up to temperature is 515-530 ℃; Open the drawing mechanism switch, adjusting the materials device rotating speed is 5 rev/mins, and the control residence time of material in burner hearth is 15min, and calcinate reclaims through discharge system and obtains the Vanadium Pentoxide in FLAKES product.Test by analysis, the Vanadium Pentoxide in FLAKES product purity reaches 98.2wt%, meets the V among the standard GB 3283-87
2O
5-98 trade mark standards.
Embodiment 3: with granularity is that 10-120 μ m ammonium meta-vanadate powder and granularity are that 10-100 μ m vanadium pentoxide powder places microwave device feed bin separately respectively after temperature is 55 ℃ of dryings, open the feeding unit switch, the by-pass cock aperture, the Vanadium Pentoxide in FLAKES that accounts for gross weight 45% is allocated in the ammonium meta-vanadate, regulating the feed auger rotating speed is 9 rev/mins, and mixture is delivered in the microwave device burner hearth; Open the microwave heating switch, regulate microwave output power to 70-75kW, with 80 ℃/min temperature rise rate mixture being warming up to temperature is 530-550 ℃; Open the drawing mechanism switch, adjusting the materials device rotating speed is 8 rev/mins, and the control residence time of material in burner hearth is 5min, and calcinate reclaims through discharge system and obtains the Vanadium Pentoxide in FLAKES product.Test by analysis, the Vanadium Pentoxide in FLAKES product purity reaches 98.5wt%, meets the V among the standard GB 3283-87
2O
5-98 trade mark standards.
Claims (1)
1. the method for a producing vanadium pentoxide by microwave calcinations of ammonium metavanadate, comprise get the raw materials ready, microwave calcined by rotary kiln, three steps of product discharging, it is characterized by:
1.1 get the raw materials ready, be the Vanadium Pentoxide in FLAKES product powder drying for standby respectively that 55 ℃ of granularities that will obtain through precipitation ammonium meta-vanadate that is 10-120 μ m and granularity are 10-100 μ m in temperature; Ammonium meta-vanadate that obtains and Vanadium Pentoxide in FLAKES are respectively charged into microwave device separately in the feed bin, regulate the feeding unit switch, the vanadium pentoxide powder that accounts for gross weight 10-50% is evenly allocated in the ammonium meta-vanadate powder, regulating the feed auger rotating speed is 3-10 rev/min, and material is delivered in the microwave device burner hearth continuously by feed auger;
1.2 microwave calcination, microwave reactor frequency are 2.45GHz, output rating is 0-80kW, and the microwave device burner hearth is a microwave dedicated ceramic pipe, is with two to add feed bin; Regulate microwave output power, with 20-100 ℃/min temperature rise rate mixture being warming up to temperature is 500-550 ℃, and the control residence time of material in burner hearth is 5-30min;
1.3 product discharging, temperature of charge to be mixed rise to the preset temperature soaking time arrive after, open drawing mechanism, adjusting the materials device rotating speed is the discharging of 2-10 commentaries on classics/clock, obtains the Vanadium Pentoxide in FLAKES product, purity is 98.5wt/%; The Vanadium Pentoxide in FLAKES quality product V among the GB3283-87 that is up to state standards
2O
5-98 trade mark standards.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101283090A CN101811734B (en) | 2010-03-22 | 2010-03-22 | Method for producing vanadium pentoxide by microwave calcinations of ammonium metavanadate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101283090A CN101811734B (en) | 2010-03-22 | 2010-03-22 | Method for producing vanadium pentoxide by microwave calcinations of ammonium metavanadate |
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| Publication Number | Publication Date |
|---|---|
| CN101811734A true CN101811734A (en) | 2010-08-25 |
| CN101811734B CN101811734B (en) | 2011-07-20 |
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|---|---|---|---|
| CN2010101283090A Expired - Fee Related CN101811734B (en) | 2010-03-22 | 2010-03-22 | Method for producing vanadium pentoxide by microwave calcinations of ammonium metavanadate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021315A (en) * | 2010-11-09 | 2011-04-20 | 化工部长沙设计研究院 | Process for calcining ammonium metavanadate for preparing powdered vanadium pentoxide |
| CN104894398A (en) * | 2015-06-16 | 2015-09-09 | 攀钢集团攀枝花钢钒有限公司 | Equipment and method for producing powdery vanadium oxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456587A (en) * | 2008-10-17 | 2009-06-17 | 芜湖人本合金有限责任公司 | Method for producing high purity vanadic anhydride |
| CN101633521A (en) * | 2009-08-17 | 2010-01-27 | 昆明理工大学 | Method for producing triuranium octoxide by microwave calcination of ammonium diuranate |
-
2010
- 2010-03-22 CN CN2010101283090A patent/CN101811734B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456587A (en) * | 2008-10-17 | 2009-06-17 | 芜湖人本合金有限责任公司 | Method for producing high purity vanadic anhydride |
| CN101633521A (en) * | 2009-08-17 | 2010-01-27 | 昆明理工大学 | Method for producing triuranium octoxide by microwave calcination of ammonium diuranate |
Non-Patent Citations (1)
| Title |
|---|
| 《无机盐工业》 20050831 曾志勇 多钒酸铵静态热分解制备粉状五氧化二钒 第20-22页 1 第37卷, 第8期 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021315A (en) * | 2010-11-09 | 2011-04-20 | 化工部长沙设计研究院 | Process for calcining ammonium metavanadate for preparing powdered vanadium pentoxide |
| CN102021315B (en) * | 2010-11-09 | 2012-05-09 | 化工部长沙设计研究院 | Process for calcining ammonium metavanadate to obtain powdery vanadium pentoxide |
| CN104894398A (en) * | 2015-06-16 | 2015-09-09 | 攀钢集团攀枝花钢钒有限公司 | Equipment and method for producing powdery vanadium oxide |
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| Publication number | Publication date |
|---|---|
| CN101811734B (en) | 2011-07-20 |
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Granted publication date: 20110720 Termination date: 20140322 |