CN1184162A - Vanadium pentoxide extracting method from stone coal vanadium ore - Google Patents
Vanadium pentoxide extracting method from stone coal vanadium ore Download PDFInfo
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- CN1184162A CN1184162A CN96118450A CN96118450A CN1184162A CN 1184162 A CN1184162 A CN 1184162A CN 96118450 A CN96118450 A CN 96118450A CN 96118450 A CN96118450 A CN 96118450A CN 1184162 A CN1184162 A CN 1184162A
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Abstract
The said vanadium pentoxide extracting method features that after partial decarbonizing, ball milling while adding 8% below salt and calcium and roast of material pellets, the ore material pellets are processed through the steps of static lixiviation in low-acid solution, solution purification, five-stage extraction, four stage reverse extraction, purification and subsequent steps. Producing V2O5 through said method has less waste gas pollution, high yield, low production cost, high product quality and no strict requirement to ore.
Description
The invention relates to a process for extracting vanadium oxide.
At present, most of vanadium extraction from stone coal in China adopts sodium salt roasting, and the process flow comprises ore crushing, decarbonization, ball milling, salt addition (the ore: the salt is 100: 13), balling, roasting at the temperature of 85-900 ℃, ore ball crushing, clarification by hot water leachate at the temperature of 80-100 ℃, crude vanadium precipitation by sulfuric acid at the temperature of 100 ℃, washing and dehydration, alkali dissolution at the temperature of 100 ℃, ammonium chloride precipitation of ammonium metavanadate, washing and dehydration of ammonium metavanadate, and firing to obtain refined vanadium. The process has the advantages of high labor intensity, high energy consumption, low yield and serious waste gas pollution. In order to eliminate serious waste gas pollution, in the last decade, many domestic research units explore various ways, for example, although the intermediate salt method developed by Zhejiang chemical industry avoids waste gas pollution caused by sodium roasting, the yield of vanadium is up to 70%, each ton of product needs to consume more than 30 tons of sulfuric acid, the cost is high, the process is complex, the equipment investment is large, and the method cannot be used for industrial production; also, as a new vanadium extraction process (patent application No. 90105503.4) of salt-free roasting normal-temperature leaching transformation extraction, which is researched by Huaishixi vanadium factory and Hunan province coal carbon research institute, the main process flow of the process is as follows: crushing ore, decarburizing, ball milling, balling, salt-free roasting at 800-1000 ℃, crushing ore balls, leaching at normal temperature-100 ℃ and pH 0-2.5, treating the ore balls with solution, adding N263, adjusting the pH to 3-6, performing transformation extraction, adding ammonium chloride for back extraction, adding ammonium chloride for transformation desorption, centrifugally drying, deaminating and firing at 250-300 ℃ to obtain the product. The process has special requirements on ores, can not bepopularized generally, and the problem of extraction and emulsification is not solved, so that the process cannot be produced normally. From abroad, the technology for extracting vanadium from carbon-containing shale is found through international online retrieval, but most of the technologies are sodium roasting, but the patent with the patent number 4115110 (method for extracting vanadium from carbon-containing vanadium ore) adopts rotary pure oxygen roasting, so that the equipment investment is large, the process requirement is high, and the method is not suitable for technical transformation by the existing vanadium plant facilities in China.
The invention aims to disclose a method for extracting vanadium from stone coal vanadium ore, which has the advantages of wide adaptability, less waste gas pollution, high yield, energy conservation, consumption reduction, low production cost and good product quality, and can effectively utilize the existing equipment of a vanadium plant for technical transformation.
The technical solution of the invention is as follows: a method for extracting vanadium from stone coal vanadium ore is characterized in that: after the crushed ore is partially decarburized, NaCl and CaCO are added according to the proportion of less than 8 percent of the weight of the ore3Simultaneously adding the vanadium powder into ore to enter a ball milling and balling process, roasting at the temperature of 750-850 ℃ after balling, directly putting roasted material balls into acid liquor with the pH of 1-3 for static leaching, adding a flocculating agent into the leached solution for purification, then extracting and back-extracting, heating the back-extracted vanadium liquid to 40-100 ℃, and performing weak alkaline treatment on the back-extracted vanadium liquidPurifying, then precipitating ammonium metavanadate, filtering, washing, drying and pyrolyzing.
NaCl and CaCO in the technical solution of the invention3The addition amount of (b) can be 5-6% of the weight of the ore.
The static pickling solution in the technical scheme of the invention can be sulfuric acid solution.
The material ball low-acid static soaking in the technical scheme of the invention can be carried out in an anti-corrosion tank or an anti-corrosion pool.
The static leaching in the technical scheme of the invention can adopt two-acid leaching and three-water washing countercurrent normal-temperature leaching.
The pH value of the static immersion liquid in the technical scheme can be 2-3.
The flocculant in the technical solution of the invention can be a No. 3 flocculant.
In the technical scheme of the invention, 8-10% of the purified liquid can be added in the extraction(R3NH)2SO4Under the conditions of (1).
The back extraction in the technical scheme of the invention can add 5-10% of Na into the extraction liquid2CO3Under the conditions of (1).
The extraction in the technical scheme of the invention can be 5 stages, and the back extraction can be 4 stages.
The vanadium liquid obtained by back extraction in the technical scheme of the invention can use NH4Adjusting the pH of OH to 6-8.
In the technical scheme of the invention, the solid-liquid ratio of static soaking is 1: 2-1: 4, preferably 1: 3.
In the technical solution of the invention (R)3NH)2SO4The amount of (c) may be 9% of the solution.
In the technical solution of the invention,Na2CO3The amount of (c) may be 8% of the solution.
By adopting the technical scheme, the invention not only reduces the waste gas pollution by two thirds, but also improves the yield by more than 20 percent compared with the original process, simplifies the process, saves a boiler, a mineral ball crusher and leaching and stirring equipment, reduces the production cost by nearly 30 percent, stably improves the product grade by 98 grades in metallurgy by 99 grades, and can even produce products of more than 99.5 percent. And the technology is improved by using the old vanadium plant equipment, and the original vanadium plant producing 100 tons every year is improved into a vanadium plant producing 150 tons every year, and the improvement cost is within 100 ten thousand yuan. Meanwhile, the method is not limited by ores and has good adaptability.
The attached drawing is a process flow chart of the invention
The invention will be further illustrated by reference to the following examples, which illustrate a process for extracting vanadium from stone coal vanadium ore, comprising the steps of:
1. decarbonization: after the stone coal vanadium ore is crushed, partial decarburization is carried out in a tube placing furnace or a fluidized bed furnace, so that 10O 0-1200 Kcal/Kg of raw ore is reduced to 500 Kcal/Kg, partial oxidation is carried out on the ore, vanadium is gradually converted from low valence to high valence, and the reaction formula is as follows:
2. ball milling: the addingproportion of the mineral is within 8 percent of the weight of the mineral, and the optimal proportion is 5 percentTo 6% NaCl and CaCO3And adding the mixture and the ore into a ball mill, and grinding the mixture into 60-mesh all-through mineral powder. NaCl, CaCO3The adding proportion of (A) is less than 3%, the conversion rate of vanadium is about 30%, the adding proportion is 5-6%, the conversion rate of vanadium is about 85%, the proportion is increased, the conversion rate is not obviously increased, and the waste gas pollution is aggravated. NaCl, CaCO3Only one of the vanadium and the vanadium is added, the proportion is controlled within 8 percent, and the conversion rate of vanadium is lower than 50 percent for most of ores.
3. Preparing balls: preparing the mineral powder balls with the diameter of 15-25 mm in a ball making machine, wherein the humidity of the balls is proper, and the ratio of the mineral powder to water is 100: 12
4. Roasting: roasting the prepared ore powder balls in a fluidized bed furnace or a flat kiln, preferably in a flat kiln, wherein the roasting time is 1-4 hours, and the best roasting time is 2-3 hours, the roasting process is a very complicated chemical reaction process, and the following effective reactions are mainly carried out:
① allowing vanadium to form soluble metavanadate and potash albite:
② vanadium formation calcium vanadate and sodium calcium vanadate:
③ the calcium magnesium oxide and quartz are combined into diopside-calcium and magnesium silicate, the roasting temperature is controlled at 750-850 deg.C, the temperature is too low, the conversion rate is low, the temperature is too high, the leaching rate is affected, preferably 830 deg.C, the average roasting conversion rate is more than 76% in laboratory, and the industrial production is more than 65%.
5. Acid leaching: and (2) directly placing the roasted material balls into an anticorrosive tank or an anticorrosive pool to carry out secondary acid leaching and tertiary water washing countercurrent normal-temperature leaching, wherein the period is about 5 days, 13 kilograms of sulfuric acid is added into water for each ton of roasted material balls, the pH value is adjusted to be 1-3, vanadium with too low pH value is converted into tetravalent vanadium, the pH value is too high, the leaching rate is reduced, preferably 2-3, the ratio of the material balls to the leaching solution is 1: 2-1: 4, the leaching rate is too low, the solution concentration is too high, the subsequent treatment is inconvenient, and preferably 1: 3. Heap leaching may also be used with a period of 45 days. In the immersion cleaning process, the material balls are still immersion cleaned without stirring. The average leaching rate in a laboratory is 92 percent, and the average leaching rate in industrial production is more than 90 percent. Because of adopting the ball-soaking, the suspension of the liquid is less, and the problem that other processes are easy to cause extraction emulsification is solved.
The main acid leaching reactions are as follows:
6. solution purification:
adding flocculating agent, preferably No. 3 flocculating agent into the vanadium liquid leached by acid, and having high precipitation speed and good purification effect. At this time, most of impurities such as Al, Fe, Ni and the like in the solution are removed, the purification loss rate is basically zero, and the reaction formula is as follows:
when al.fe is hydrolyzed to precipitate as hydroxide colloid, si.p.as impurities in the solution are also adsorbed to different degrees to produce their precipitates to be removed. The amount of flocculant added is negligible to the weight of the solution.
7. And (3) extraction:
adding (R) accounting for 8-10%, preferably 9% of the vanadium solution into the purified vanadium-containing solution3NH)2SO4Performing five-stage extraction, wherein the pH value of the solution is between 1 and 4, preferably between 2 and 3,the extraction rate can reach more than 99 percent, and the reaction formula is as follows:
3(R3NH)2SO4+HV10O28 5(R3NH)6HV10O28+3SO4
8. back extraction: adding Na accounting for 5-10%, preferably 8%, of the extraction solution into the extraction solution2CO3Adjusting the pH value to 6-8.5 to perform four-stage back extraction, wherein the back extraction rate reaches 99.8 percent, and the reaction formula is as follows:
9. and (3) purification:
heating vanadium liquid obtained by back extraction with NH4Adjusting the pH value of OH to 6-8, and standing for 6-10 hours to hydrolyze and precipitate the alkali metal. The heating heat comes from a tube placing furnace in the decarburization process, and the temperature is controlled to be 40-100 ℃.
10. Precipitating ammonium metavanadate, filtering the purified vanadium solution, adjusting the value to slightly alkaline, heating to destroy yellow heteropoly acid, and adding ammonium chloride to precipitate the ammonium metavanadate. The dosage of ammonium chloride is more than that required by the reaction, generally 1.2T of ammonium chloride is added into one ton of vanadium pentoxide, and the precipitation rate reaches more than 99.9 percent.
11. Filtering, washing and spin-drying:
and filtering the ammonium metavanadate by using a filter bag, washing by using clear water after filtering, and drying by using a drying machine after washing.
12. Drying and pyrolyzing:
calcining the obtained ammonium metavanadate in a burning cylinder at the temperature of 450-550 ℃, and decomposing to obtain V2O5. The thermal decomposition process is generally carried out in the air, and is continuously stirred to avoid incomplete oxidation, and the vanadium pentoxide obtained by decomposition is golden yellow or brick red powder, and the purity is more than or equal to 99%.
The invention uses low sodium and calcium to roast weak acid normal temperature material ball static leaching extraction process, breaks through the forbidden zone that the vanadium extraction from stone coal can only be pure sodium roasting or calcification roasting, but can not be done with sodium and calcium roasting at the same time and breaks through the routine that the material ball must be crushed and leached, through the industrialized test production, the salt consumption is reduced from 13% to about 5%, the waste gas pollution is reduced by two thirds, the total yield is about 60%, and is improved by more than 20% compared with the original process. The process is greatly simplified, particularly a steam boiler and 15 sets of crushing, leaching and stirring equipment and a plate-and-frame filter press which are 110KW in total are omitted, the actual workshop cost is reduced to 2.86 ten thousand yuan/ton from the original 4.2 ten thousand yuan/ton, the yield is increased by one third, namely the yield reaches 150 tons/year from the original 100 tons/year, the product quality is improved by one step, the metallurgy 98 grade is stably improved to more than 99 grade, even more than 99.5 percent of products can be produced, and the products analyzed by a research institute of nonferrous metals in Hunan province reach 99.7 percent. The invention has no strict requirement on ore, has wide adaptability, can save about 70 percent of investment compared with the reconstruction of the plant by utilizing the device to carry out technical reconstruction on the existing vanadium plant facilities, and has the significance of popularization.
Claims (15)
1. A method for extracting vanadium from stone coal vanadium ore is characterized in that: after partial decarbonization of the crushed ore, NaCl and CaCO are added in a proportion of less than 8 percent of the weight of the ore3Adding the vanadium powder into ore, performing ball milling and balling, roasting at the temperature of 750-850 ℃ after balling, directly leaching the roasted material balls in acid liquor with the pH value of 1-3, purifying the solution obtained by static leaching by adding a flocculating agent, extracting and back-extracting, heating the vanadium liquid obtained by back-extraction to 40-100 ℃, purifying the vanadium liquid under alkalescence, precipitating ammonium metavanadate, filtering, washing, spin-drying, drying and pyrolyzing.
2. The method of claim 1, wherein the method comprises extracting vanadium from stone coal vanadium ore with NaCl and CaCO3The addition amount of (A) is 5-6% of the weight of the ore.
3. A process according to claim 1 or claim 2 for extracting vanadium from stone coal vanadium ore. It is characterized in that the roasting temperature is 830 ℃.
4. A method of extracting vanadium from vanadium stone coal mine according to claim 1, characterized in that the pellet low acid leaching is carried out in an anti-corrosion tank or pool.
5. The method for extracting vanadium from stone coal vanadium ore according to claim 1, characterized in that the static leaching adopts two-acid leaching and three-water washing countercurrent normal temperature leaching.
6. The method for extracting vanadium from stone coal vanadium ore according to claim 1, wherein the pH value of the still immersion liquid is 2-3.
7. The method for extracting vanadium from stone coal vanadium ore according to claim 1, characterized in that the flocculant is a No. 3 flocculant.
8. The method for extracting vanadium from vanadium-bearing coal ore according to claim 1, characterized in that the extraction is five-stage and the back extraction is four-stage.
9. The method for extracting vanadium from stone coal vanadium ore according to claim 1 or 8, characterized in that the extraction is carried out by adding 8-10% (R) into the purified solution3NH)2SO4Under the conditions of (1).
10. The method for extracting vanadium from stone coal vanadium ore according to claim 1 or 3, characterized in that the back extraction is to add 5-10% of Na into the extraction liquid2Co3Under the conditions of (1).
11. The method for extracting vanadium from stone coal vanadium ore according to claim 1, wherein the pH value of the vanadium solution obtained by back extraction is NA4Adjusting the pH of OH to 6-8.
12. The method for extracting vanadium from stone coal vanadium ore according to claim 1, characterized in that the solid-to-liquid ratio of the static leaching is 1: 2-1: 4.
13. The method of claim 17, wherein the solid-to-liquid ratio of the static leaching is 1: 3.
14. The method of claim 9, wherein (R) is a vanadium extraction from stone coal vanadium ore3NH)2SO4The amount of (B) added was 9% of the solution.
15. The method for extracting vanadium from stone coal vanadium ore according to claim 10, characterized in that Na2CO3The amount of (B) added is 8% of the solution.
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| CN96118450A CN1057130C (en) | 1996-12-06 | 1996-12-06 | Vanadium pentoxide extracting method from stone coal vanadium ore |
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| CN96118450A CN1057130C (en) | 1996-12-06 | 1996-12-06 | Vanadium pentoxide extracting method from stone coal vanadium ore |
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| CN1057130C CN1057130C (en) | 2000-10-04 |
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| CN100360428C (en) * | 2006-06-22 | 2008-01-09 | 姚明峰 | Method for picking up vanadium pentexide from layer silicate without oxidation in furnace |
| CN100519425C (en) * | 2007-05-25 | 2009-07-29 | 攀钢集团攀枝花钢铁研究院 | Process of extracting vanadium pentoxide from coal gangue |
| CN101062783B (en) * | 2006-04-30 | 2010-05-12 | 邱宏麒 | Environment-friendly type technique for vanadium extraction of stone coal |
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| CN101215647B (en) * | 2008-01-16 | 2010-06-09 | 中南大学 | Roasting technique for extracting vanadium from stone coal vanadium ore |
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| CN1049141A (en) * | 1989-08-01 | 1991-02-13 | 化学工业部天津化工研究院 | Produce the sinter process of Vanadium Pentoxide in FLAKES |
| CN1040132C (en) * | 1992-08-12 | 1998-10-07 | 湖南省洪江市黔城钒厂 | Settling process for extracting vanadium from bone coal |
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| CN100360428C (en) * | 2006-06-22 | 2008-01-09 | 姚明峰 | Method for picking up vanadium pentexide from layer silicate without oxidation in furnace |
| CN1899971B (en) * | 2006-07-01 | 2011-08-03 | 谢更生 | Method for extracting V2O5 from stone coal vanadium ore |
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