CN1752022A - Method of extracting vanadium pentoxide from vanadium ore - Google Patents
Method of extracting vanadium pentoxide from vanadium ore Download PDFInfo
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- CN1752022A CN1752022A CNA2005100320123A CN200510032012A CN1752022A CN 1752022 A CN1752022 A CN 1752022A CN A2005100320123 A CNA2005100320123 A CN A2005100320123A CN 200510032012 A CN200510032012 A CN 200510032012A CN 1752022 A CN1752022 A CN 1752022A
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Abstract
A process for extracting V2O5 from vanadium ore includes such steps as calcining for calcifying, extracting in deluted acid, purifying V solution, ion exchange and thermodecompsing for deammonifying. Its advantages are high purity (more than 98%) and high recovery rate (more than 62%).
Description
Technical Field
The invention relates to a method for extracting vanadium pentoxide from vanadium ore.
Background
At present, most of vanadium pentoxide extracted from vanadium ore at home is roasted by sodium treatment, and the technological process comprises the steps of ore crushing, decarbonization, ball milling, salt addition (the ratio of ore to salt is 100: 13), balling, roasting at 850-900 ℃, ore ball crushing, clarification by hot water leachate at 80-100 ℃, precipitation of primary vanadium by sulfuric acid at 100 ℃, washing and dehydration, alkali dissolution at 100 ℃, precipitation of ammonium metavanadate by ammonium chloride, washing and dehydration of ammonium metavanadate, and ignition of ammonium metavanadate to obtain refined vanadium. The process has the advantages of high labor intensity, high energy consumption, low vanadium yield and serious waste gas pollution.
Disclosure of Invention
The invention aims to provide a method for extracting vanadium pentoxide from vanadium ore, which has the advantages of less waste gas pollution, high vanadium recovery rate, low consumption, low energy consumption, good product quality and strong ore adaptability.
The technical solution of the invention is as follows: a process for extracting vanadium pentoxide from vanadium ore includes such steps as calcine by calcification, immersing in diluted acid, purifying vanadium liquid, ion exchange and thermal decomposition to remove ammonia.
Calcification roasting: mixing vanadium-containing stone coal and vanadium-containing oxidized ore according to the weight ratio of 1: 1-1: 3, crushing to 60-100 meshes, adding 5-10% of quicklime by the total weight of the ore, stirring uniformly, adding 0.3-0.8% of additive by the total weight of the ore, wherein the additive is ethyl heteropolyacid sodium phosphate, balling, feeding into a furnace, controlling the furnace temperature to roast at 900-980 ℃ to obtain the cooked ball, and the color of the cooked ball is grey white or green yellow.
In the oxidizing atmosphere in the furnace, minerals are fully decomposed, vanadium ions are converted from low valence to high valence, and then the vanadium ions and active calcium are combined to generate calcium vanadate. The main chemical reactions are expressed as follows:
in addition, main element components such as silicon, phosphorus, aluminum and the like contained in the vanadium ore respectively generate precipitate substances such as calcium silicate, calcium phosphate, calcium metaaluminate and the like when meeting CaO under the high-temperature condition, and harmful gas is not generated in the calcification roasting process, so that the environmental pollution is not caused.
Leaching with dilute acid: putting the cooked balls into a pool, soaking the balls in dilute acid at normal temperature, wherein the pH value is 2.5-3.0, and generally adopting a three-soaking three-washing operation mode, and each pool needs about 3 to 5 days.
Purifying the vanadium liquid: pumping the leached mother liquor into a settling tank, wherein the impurity components in the mother liquor, such As Al, Fe, Ni, Si, As, Cr, Cd and the like, can generate precipitate only by adjusting the pH value and adding a certain amount of purifying agent, and then naturally settling. The purifying agent is a mixture of sodium hydroxide and sodium carbonate, and the adding amount of the purifying agent is determined by the content of metal ions and the pH value of the mother liquor water.
Ion exchange: adjusting the pH value of the settled mother liquor water to 2.5-3.0, entering an ion exchange column for adsorption exchange to separate vanadium and water, stopping adsorption after resin absorption reaches saturation, adding a stripping liquid to strip vanadium, wherein the stripping liquid is a sodium hydroxide solution, then putting the stripping liquid with high vanadium concentration into a vanadium precipitation tank, adding ammonium chloride, and stirring to generate ammonium metavanadate, wherein the addition amount of the ammonium chloride is more than the dosage required by reaction; the tail water after ion exchange has weak acidity and a pH value of 3.0-4.0, and is used for soaking cooked balls for recycling.
Pyrolysis deamination: the ammonium metavanadate after being released and precipitated is centrifugally dehydrated and then enters an electric oven to be deaminated at the temperature of 500-600 ℃ to prepare V2O5。
Compared with the prior art, the invention has the following advantages:
1. in the prior art, the stone coal sodium modification vanadium extraction pollution source has four aspects: firstly, a large amount of chlorine gas and sulfur dioxide gas are generated in the roasting process, and acid rain is easily formed; secondly, a large amount of sulfuric acid-containing wastewater is generated during the crude vanadium boiling process, and the wastewater is inconvenient to recycle due to high water temperature; thirdly, the waste residues contain a large amount of mineral salts (oxides) and other element impurities which are insoluble in water, so that soil salinization is easily caused; fourthly, the raw materials are crushed, stirred and cooked during soaking, and a large amount of generated slurry needs to be stored in a large number of places and is difficult to treat. Therefore, compared with the sodium roasting process, the novel calcification roasting process has the following advantages: firstly, the flue gas is free of chlorine gas, calcium has a sulfur fixing effect, sulfur dioxide gas in the flue gas is few, no pungent smell exists, and no damage is caused to peripheral crops; the pickling acid solution is recycled, no acid water is discharged, only a small amount of washing water for back flushing the resin is discharged, the water is weakly acidic, the pH value is 4.0-5.0, and the pickling acid solution can reach the standard of farmland irrigation water after being added with a small amount of lime for neutralization and precipitation and is used as the farmland irrigation water; thirdly, the waste slag does not contain chloride, harmful elements in the slag are lower than the emission standard, and the waste slag contains higher calcium and is a better filling material for cement production; and fourthly, the process basically has no slurry overflow phenomenon.
2. The tail water after ion exchange is recycled, so that the cost can be saved, and meanwhile, the soil acidification caused by the discharge of acidic water is avoided, and the environment protection is facilitated.
3. V of the invention2O5The roasting conversion rate is more than 66%, the leaching rate is more than 98%, the purification recovery rate is more than 98%, the ion exchange recovery rate is more than 99%, the pyrolysis deamination recovery rate is more than 98%, the total recovery rate is more than 62%, and compared with the prior art, the method has the advantages that the roasting conversion rate is more than 66%, the leaching rate is more than 98%, the purification recovery rate is more than 98%, the2O5The conversion rate is improved by 20 percent, and the total recovery rate is improved by 20 percent.
4. The discharge of the three wastes meets the environmental protection requirement.
5. Simple operation, wide roasting temperature range and loose heat productivity ratio of furnace burden.
6. The purity of the product is more than 98.0 percent.
Drawings
FIG. 1 is a process flow diagram of the present invention
Detailed Description
The present invention will be further described with reference to the following examples, in which a process for extracting vanadium pentoxide from vanadium ore is carried out by the following steps:
1. crushing: the vanadium-containing stone coal and vanadium-containing oxidized ore are crushed in a crusher to obtain 60-100 meshes of ore powder.
2. Preparing balls: mixing vanadium-containing stone coal mineral powder and vanadium-containing oxidized mineral powder according to the weight ratio of 1: 2, adding limestone powder accounting for 8% of the total weight of the mineral powder and sodium ethyl heteropolyacid phosphate accounting for 0.5% of the total weight of the mineral powder, fully mixing in a grinding mixer, and preparing into mineral powder balls in a ball forming mill.
3. Roasting: and roasting the prepared ore powder balls in a fluidized bed furnace or a flat cellar, preferably in the flat cellar, wherein the roasting time is 2-8 hours, and the best roasting time is 4-6 hours to prepare the cooked balls. The roasting temperature is controlled to be 900-980 ℃, the temperature is too low, the conversion rate is low, the temperature is too high, the leaching rate is influenced, the best is 950 ℃, the average roasting conversion rate is more than 70 percent in a laboratory, and the industrial production is more than 66 percent.
4. Acid leaching: crushing the cooked balls in a double-roller machine, entering a soaking pool, adding 3% hydrochloric acid and 5% sulfuric acid, controlling the pH value to be 2.5-3.0, carrying out acid leaching, adopting a three-leaching and three-washing operation mode, wherein each pool needs 3-5 times, three-leaching water enters a natural settling pool, and the three-washing water is stored and returned to the soaking pool for three-leaching water recycling.
5. Purifying the vanadium liquid: pumping the leached mother liquor into a clarifying tank, determining the addition amount of a mixture of sodium hydroxide and sodium carbonate according to the content of metal ions obtained by elements such As Al, Fe, Ni, Si, As, Cr, Cd and the like in the impurity components in the mother liquor and the pH value of the mother liquor, adding the mixture of sodium hydroxide and sodium carbonate to enable the metal ions to generate precipitate substances, and naturally clarifying to obtain the clarified mother liquor.
6. Ion exchange: adjusting the pH value of the settled mother liquor to 2.5-3.0, entering an ion exchange column for adsorption exchange to separate vanadium and water, stopping adsorption after resin is saturated, adding a stripping liquid to strip vanadium, and then putting the stripping liquid with high vanadium concentration into a vanadium precipitation tank; tail water after ion exchange is weakly acidic, the pH value is 3.0-4.0, and the tail water is used for soaking cooked balls for recycling.
7. And (3) vanadium precipitation: and adding ammonium chloride with a dosage exceeding that required by the reaction into a vanadium precipitation tank, stirring to generate ammonium metavanadate, and removing washing water through a centrifuge to obtain the dehydrated ammonium metavanadate.
8. Pyrolysis deamination: the dehydrated ammonium metavanadate is sent into an electric oven to be subjected to deammoniation at the temperature of 500-600 ℃ to prepare V2O5。
Claims (1)
1. The method for extracting vanadium pentoxide from vanadium ore is characterized by comprising five processes of calcification roasting, dilute acid leaching, vanadium liquid purification, ion exchange and pyrolysis deamination:
a. calcification roasting: mixing vanadium-containing stone coal and vanadium-containing oxidized ore according to the weight ratio of 1: 1-1: 3, crushing to 60-100 meshes, adding quicklime accounting for 5-10% of the total weight of the ore, stirring uniformly, adding an additive accounting for 0.3-0.8% of the total weight of the ore, wherein the additive is ethyl heteropolyacid sodium phosphate, balling and feeding into a furnace, and roasting at 900-980 ℃ to obtain a cooked ball, wherein the color of the cooked ball is grey white or green yellow;
b. leaching with dilute acid: putting the cooked balls into a pool, soaking the balls in dilute acid at normal temperature, wherein the pH value is 2.5-3.0, generally adopting a three-soaking three-washing operation mode, and each pool needs about 3 to 5 days;
c. purifying the vanadium liquid: pumping the leached mother liquor into a settling tank, wherein the impurity components in the mother liquor, such As Al, Fe, Ni, Si, As, Cr, Cd and the like, can generate precipitate only by adjusting the pH value and adding a certain amount of purifying agent, and then naturally settling; the purifying agent is a mixture of sodium hydroxide and sodium carbonate, and the adding amount of the purifying agent is determined by the content of metal ions and the pH value of the mother liquor water;
d. ion exchange: adjusting the pH value of the settled mother liquor water to 2.5-3.0, entering an ion exchange column for adsorption exchange to separate vanadium and water, stopping adsorption after resin absorption reaches saturation, adding a stripping liquid to strip vanadium, wherein the stripping liquid is a sodium hydroxide solution, then putting the stripping liquid with high vanadium concentration into a vanadium precipitation tank, adding ammonium chloride, and stirring to generate ammonium metavanadate, wherein the addition amount of the ammonium chloride is more than the dosage required by reaction; tail water after ion exchange has weak acidity and a pH value of 3.0-4.0, and is used for soaking cooked balls for recycling;
e. pyrolysis deamination: the ammonium metavanadate after being released and precipitated is centrifugally dehydrated and then enters an electric oven to be deaminated at the temperature of 500-600 ℃ to prepare V2O5。
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Cited By (19)
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|---|---|---|---|---|
| CN100375716C (en) * | 2006-08-14 | 2008-03-19 | 中国铝业股份有限公司 | Method of recovering V2O5 from Bayer process mother liquid |
| CN100425712C (en) * | 2006-11-23 | 2008-10-15 | 新疆汇友矿业设计研究院(有限公司) | Technique for extracting vanadium pentoxide by the pulp resin method |
| CN100519425C (en) * | 2007-05-25 | 2009-07-29 | 攀钢集团攀枝花钢铁研究院 | Process for Extracting Vanadium Pentoxide from Stone Coal Mine |
| CN101062783B (en) * | 2006-04-30 | 2010-05-12 | 邱宏麒 | Environment-friendly type technique for vanadium extraction of stone coal |
| CN101274778B (en) * | 2008-05-07 | 2010-06-02 | 紫金矿业集团股份有限公司 | Method for extracting vanadic anhydride from stone coal |
| CN101760651A (en) * | 2010-03-04 | 2010-06-30 | 中南大学 | Process for extracting vanadium by acid leaching of stone coal |
| CN101289705B (en) * | 2007-04-20 | 2010-07-14 | 北京化工大学 | A method for extracting vanadium from iron-making waste slag of vanadium ore |
| CN101838749A (en) * | 2010-06-10 | 2010-09-22 | 中南大学 | Ion exchange extraction vanadium method of vanadium-containing solution |
| CN101265524B (en) * | 2008-04-17 | 2010-10-06 | 武汉科技大学 | Method for extracting V2O5 from stone coal |
| CN101215648B (en) * | 2008-01-18 | 2011-12-28 | 贵州义信矿业有限公司 | Composite additive used for extracting vanadium from vanadium stone coal ore and using method thereof |
| CN102560090A (en) * | 2012-01-05 | 2012-07-11 | 宣恩县青龙超群矿业有限责任公司 | Method for enriching vanadium and selenium in process of producing cement ingredients by using boiling furnace |
| CN102560155A (en) * | 2012-02-22 | 2012-07-11 | 广西冶金研究院 | Method for extracting vanadium from stone coal vanadium ore by using calcium compound additive |
| CN103255287A (en) * | 2013-05-03 | 2013-08-21 | 湖南省矿产测试利用研究所 | A process for extracting vanadium pentoxide from stone coal vanadium ore |
| CN103627892A (en) * | 2012-08-28 | 2014-03-12 | 三穗县恒峰矿业有限公司 | Method for extracting vanadium from stone coal by utilizing fluidized bed |
| CN104131161A (en) * | 2014-08-13 | 2014-11-05 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting soluble vanadium from calcified clinker through sulfuric acid leaching and method for testing soluble vanadium and roasting conversion rate |
| CN104630483A (en) * | 2015-01-13 | 2015-05-20 | 漯河兴茂钛业股份有限公司 | Alkaline leaching vanadium precipitation method for comprehensive waste denitration catalyst utilization |
| CN109706329A (en) * | 2018-12-27 | 2019-05-03 | 大连博融新材料有限公司 | A kind of method that extracting vanadium from stone coal prepares ammonium metavanadate |
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| CN114480883A (en) * | 2021-12-16 | 2022-05-13 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadium pentoxide by synergistically removing silicon and chromium in vanadium solution through nickel ions |
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| CN1089237A (en) * | 1992-03-23 | 1994-07-13 | 胡良 | Roasting process for directly preparing vanadium white |
| CN1065494A (en) * | 1992-05-16 | 1992-10-21 | 湖南省煤炭科学研究所 | A kind of novel method of from contain vanadium solution, extracting Vanadium Pentoxide in FLAKES |
| RU2080401C1 (en) * | 1995-07-20 | 1997-05-27 | Акционерное общество открытого типа "Ванадий-Тулачермет" | Method of extracting vanadium from converter slag |
| CN1126821C (en) * | 2001-08-14 | 2003-11-05 | 韦文虎 | Process for extracting vanadium |
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| CN100375716C (en) * | 2006-08-14 | 2008-03-19 | 中国铝业股份有限公司 | Method of recovering V2O5 from Bayer process mother liquid |
| CN100425712C (en) * | 2006-11-23 | 2008-10-15 | 新疆汇友矿业设计研究院(有限公司) | Technique for extracting vanadium pentoxide by the pulp resin method |
| CN101289705B (en) * | 2007-04-20 | 2010-07-14 | 北京化工大学 | A method for extracting vanadium from iron-making waste slag of vanadium ore |
| CN100519425C (en) * | 2007-05-25 | 2009-07-29 | 攀钢集团攀枝花钢铁研究院 | Process for Extracting Vanadium Pentoxide from Stone Coal Mine |
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| CN101265524B (en) * | 2008-04-17 | 2010-10-06 | 武汉科技大学 | Method for extracting V2O5 from stone coal |
| CN101274778B (en) * | 2008-05-07 | 2010-06-02 | 紫金矿业集团股份有限公司 | Method for extracting vanadic anhydride from stone coal |
| CN101760651A (en) * | 2010-03-04 | 2010-06-30 | 中南大学 | Process for extracting vanadium by acid leaching of stone coal |
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| CN102560090B (en) * | 2012-01-05 | 2013-10-02 | 宣恩县青龙超群矿业有限责任公司 | Method for enriching vanadium and selenium in process of producing cement ingredients by using boiling furnace |
| CN102560155A (en) * | 2012-02-22 | 2012-07-11 | 广西冶金研究院 | Method for extracting vanadium from stone coal vanadium ore by using calcium compound additive |
| CN103627892A (en) * | 2012-08-28 | 2014-03-12 | 三穗县恒峰矿业有限公司 | Method for extracting vanadium from stone coal by utilizing fluidized bed |
| CN103255287A (en) * | 2013-05-03 | 2013-08-21 | 湖南省矿产测试利用研究所 | A process for extracting vanadium pentoxide from stone coal vanadium ore |
| CN104131161A (en) * | 2014-08-13 | 2014-11-05 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting soluble vanadium from calcified clinker through sulfuric acid leaching and method for testing soluble vanadium and roasting conversion rate |
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| CN104630483A (en) * | 2015-01-13 | 2015-05-20 | 漯河兴茂钛业股份有限公司 | Alkaline leaching vanadium precipitation method for comprehensive waste denitration catalyst utilization |
| CN109706329A (en) * | 2018-12-27 | 2019-05-03 | 大连博融新材料有限公司 | A kind of method that extracting vanadium from stone coal prepares ammonium metavanadate |
| CN109957657A (en) * | 2019-03-22 | 2019-07-02 | 昆明理工大学 | A method for simultaneous resource utilization of iron, sodium and aluminum from red mud |
| CN109957657B (en) * | 2019-03-22 | 2020-11-24 | 昆明理工大学 | A method for simultaneous resource utilization of iron, sodium and aluminum from red mud |
| CN114480883A (en) * | 2021-12-16 | 2022-05-13 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadium pentoxide by synergistically removing silicon and chromium in vanadium solution through nickel ions |
| CN114480883B (en) * | 2021-12-16 | 2023-11-21 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadium pentoxide by removing silicon and chromium in vanadium solution through nickel ion cooperation |
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