CN1003079B - Technology for concentration and extraction of vanadium penta oxide from a dilute vanadium-contg. solution - Google Patents
Technology for concentration and extraction of vanadium penta oxide from a dilute vanadium-contg. solution Download PDFInfo
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- CN1003079B CN1003079B CN87101977A CN87101977A CN1003079B CN 1003079 B CN1003079 B CN 1003079B CN 87101977 A CN87101977 A CN 87101977A CN 87101977 A CN87101977 A CN 87101977A CN 1003079 B CN1003079 B CN 1003079B
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Abstract
The present invention proposes a technology for enriching and extracting vanadium pentoxide from vanadium-containing diluted solutions. The technology adopts alkali to adjust the pH value and adopts cupric salt as precipitating agents for causing vanadium ions to generate copper vanadate precipitates for enriching vanadium, uses sodium hydroxide to dissolve and purify vanadium and uses ammonium salt to generate poly-ammonium vanadate which is roasted and made into vanadium pentoxide finished products. The technology is mainly suitable for the enrichment and the extraction of leach solutions after the roasting of lower-grade vanadium-containing ores , vanadium-containing solutions discharged by vanadium smelting factories and leach solutions of vanadium-containing waste catalysts.
Description
The present invention be a kind of from contain the vanadium dilute solution enrichment extract the technology of Vanadium Pentoxide in FLAKES.
Patent searching finds to disclose among the Japanese clear 58-110428 a kind of " reclaiming the method for vanadium from the dilute solution that contains vanadium ".This method is introduced: in containing the liquid effluent of vanadium, adding excessive lime concerning vanadium, the pH value of solution is adjusted to 8-11, make the vanadic acid calcium deposit of generation, add entry after the filtration and make it be dissolved as the vanadic acid calcium aqueous solution, be blown into carbonic anhydride to solution, when treating that pH value reaches 6.5-8, a kind of with caustic alkali or carbonic acid alkali transfers pH value to make calcium deposit to 8-10 again, in the aqueous solution that filters out, add mineral acid, make poly-vanadic acid separate out separation.The problem that this method exists is that (1) is though carbonic anhydride is a burning and gas-exhausting, cost is low, but general production scene is difficult for satisfying, and (2) are adopted and are blown into carbonic anhydride, must build corresponding device thereof, as reaction tower etc., make the recovery system bulky complex, (3) make precipitation agent with lime, though inexpensive, but do not recycle, can cause the expense that reclaims vanadium to increase.
China adopts the ammonium salt vanadium extracting methods more in Vanadium Pentoxide in FLAKES is produced at present, be applicable to more and contain the high solution of vanadium, and to containing the vanadium dilute solution (as low product navajoite stone roasting leach liquor, the vanadium-containing water that vanadium smelter is discharged, or the leach liquor of vanadium-containing wasting catalyst) vanadium in, though can make the vanadium ion enrichment with extraction process or ion exchange method in the laboratory at present, because complex process, the expense height, and be not suitable for industrialness production.
The objective of the invention is to study a kind of from contain the vanadium dilute solution enrichment extract the technology of Vanadium Pentoxide in FLAKES, make the vanadium that contains in the vanadium dilute solution obtain recycling with the industrial production form, improve resource utilization, increase the economic benefit of factory.
The present invention is in the dilute solution that contains vanadium 0.05-1%, particularly at low grade vanadium ore leach liquor, vanadium smelter contain the vanadium liquid effluent, in the vanadium-containing wasting catalyst leach liquor, bivalent cupric ion (providing by soluble copper salt) is provided, when transferring pH value 7-8 with alkali, generate vanadic acid copper, cupric silicate, the copper hydroxide co-precipitation, make vanadium be able to enrichment, every liter of remaining vanadium is less than 50ppm in the solution after the filtration, be deposited under normal temperature or the 50-60 ℃ condition, when transferring pH value 1.5-2 with mineral acid, the Vanadium Pentoxide in FLAKES crude product is separated out in hydrolysis, and the weight ratio that adds bivalent cupric ion and Vanadium Pentoxide in FLAKES in the solution is 3.6: 1.
Stay cupric ion in the solution and can return and make enrichment vanadium usefulness, copper is recycled.In the Vanadium Pentoxide in FLAKES crude product, add the caustic soda dissolving when pH value is 11-13, make impurity copper generate the elimination of copper hydroxide precipitation, in solution, add ammonium chloride, transfer pH value by 2.3 o'clock with hydrochloric acid, when being warmed to 90-95 ℃, generate poly-ammonium vanadate precipitation, will gather ammonium vanadate roasting under 600-700 ℃ of condition after the filter, promptly obtain content at the Vanadium Pentoxide in FLAKES finished product more than 98%.
Advantage of the present invention is, technical process is short, and equipment is simple, and precipitation agent is cheap, can be recycled less investment, instant effect.
Embodiment 1
Claim to contain centesimal navajoite stone 1000 grams of vanadium, pulverize the back and add sodium-chlor 90 grams, yellow soda ash 10 grams add water and mix thoroughly on a small quantity and make piece, and 850 ℃ of roastings 2 hours, pulverized cold back, leaches with 10 times of clear water and filter, and leach liquor contains vanadium 0.5 for every liter and restrains.Stir and add 37 milliliters of 20% copper-baths, transfer pH value to 7.5 with sodium hydroxide, generate vanadic acid copper copper hydroxide, the cupric silicate precipitation, after the filtration, filtrate can be returned and do precipitation usefulness, add hydrochloric acid and transfer pH value to 1.5-2 in throw out, water at normal temperature solves the Vanadium Pentoxide in FLAKES crude product, after the filtration, in the Vanadium Pentoxide in FLAKES crude product, add the caustic soda soln dissolving, pH value makes impurity copper generate copper hydroxide precipitation, elimination during to 11-13, in filtrate, add 10 gram ammonium chlorides, heat to 90 ℃, transfer pH value 2.3, generate poly-ammonium vanadate precipitation with hydrochloric acid, filtering the back is placed on throw out in the luxuriant good fortune stove, when being warmed to 600 ℃, roasting 1 hour promptly obtains vanadiumcontent at the Vanadium Pentoxide in FLAKES finished product more than 98%.
Embodiment 2
At present, in the vanadium-containing water that vanadium smelter is discharged, every liter contains about 0.3 gram of vanadium.Get 1000 milliliters of vanadium-containing waters, add 17 milliliters of 20% copper-baths, transfer pH value to equal at 7.5 o'clock with sodium hydroxide solution, generate vanadic acid copper precipitation, filter the back and use the dissolving with hydrochloric acid throw out, be warmed to 60 ℃, the accent pH value is 15-2, and the Vanadium Pentoxide in FLAKES crude product is separated out in hydrolysis.Filter the back taking precipitate, add the caustic soda soln dissolving, when pH value reaches 11-13, generate the elimination of copper hydroxide precipitation, add 5 gram ammonium chlorides in the filtrate, heat to 95 ℃, transfer pH value to 2.3 with hydrochloric acid, generate poly-ammonium vanadate precipitation, poly-ammonium vanadate was placed in 600 ℃ of smelting furnaces roasting 1 hour, promptly obtain the Vanadium Pentoxide in FLAKES finished product.
Embodiment 3
Vanadium-containing wasting catalyst pulverize, water logging, the solution that every liter of concentration is contained vanadium 5-10 gram can directly add the ammonium chloride vanadium extraction.In order to improve the extraction yield of vanadium, adopt the water washing of 15 times of volumes, every liter contains vanadium 0.1-1 gram.Adopt the method for embodiment 1 to extract Vanadium Pentoxide in FLAKES to this vanadium dilute solution that contains.
Claims (4)
1, a kind of being used for extracted the technology of Vanadium Pentoxide in FLAKES from containing the enrichment of vanadium dilute solution, with regulating pH value, ammonium salt process is produced poly-ammonium vanadate, Vanadium Pentoxide in FLAKES is made in roasting, it is characterized in that transferring the solution pH value with sodium hydroxide is 7-8, make precipitation agent with bivalent cupric ion, generate vanadic acid copper precipitation, use the dissolving with hydrochloric acid throw out, when pH value is 1.5-2, the Vanadium Pentoxide in FLAKES precipitation is separated out in hydrolysis, realize that vanadium separates with copper, make the vanadium in the solution obtain enrichment, with alkaline solution dissolution precipitation thing, when PH is 11-13, remove the impurity copper in the Vanadium Pentoxide in FLAKES.
2, technology according to claim 1, it is characterized in that generating the sedimentary best pH value of vanadic acid copper is 7.5.
3, technology according to claim 1 is characterized in that bivalent cupric ion is provided by cupric chloride, copper sulfate, cupric nitrate.
4, technology according to claim 1, the optimum weight ratio that it is characterized in that cupric ion and Vanadium Pentoxide in FLAKES is 3.6: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87101977A CN1003079B (en) | 1987-03-16 | 1987-03-16 | Technology for concentration and extraction of vanadium penta oxide from a dilute vanadium-contg. solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87101977A CN1003079B (en) | 1987-03-16 | 1987-03-16 | Technology for concentration and extraction of vanadium penta oxide from a dilute vanadium-contg. solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN87101977A CN87101977A (en) | 1987-08-26 |
| CN1003079B true CN1003079B (en) | 1989-01-18 |
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ID=4813707
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN87101977A Expired CN1003079B (en) | 1987-03-16 | 1987-03-16 | Technology for concentration and extraction of vanadium penta oxide from a dilute vanadium-contg. solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1003079B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102121068B (en) * | 2011-04-08 | 2014-06-11 | 北京矿冶研究总院 | Method for preparing vanadium pentoxide |
| CN102534267A (en) * | 2012-02-06 | 2012-07-04 | 四川省达州钢铁集团有限责任公司 | Vanadium extracting method |
| CN103130278B (en) * | 2013-02-28 | 2014-07-23 | 安徽工业大学 | Copper vanadate nanoneedles and preparation method thereof |
| CN110803714A (en) * | 2019-12-17 | 2020-02-18 | 中南大学 | Method for producing vanadium pentoxide by vanadium-containing solution |
| CN116375084B (en) * | 2023-05-30 | 2023-08-01 | 寰泰储能科技股份有限公司 | Preparation method of vanadium pentoxide |
-
1987
- 1987-03-16 CN CN87101977A patent/CN1003079B/en not_active Expired
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| Publication number | Publication date |
|---|---|
| CN87101977A (en) | 1987-08-26 |
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