CN102251113A - Method for purifying vanadium leaching solution - Google Patents
Method for purifying vanadium leaching solution Download PDFInfo
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- CN102251113A CN102251113A CN2011101941812A CN201110194181A CN102251113A CN 102251113 A CN102251113 A CN 102251113A CN 2011101941812 A CN2011101941812 A CN 2011101941812A CN 201110194181 A CN201110194181 A CN 201110194181A CN 102251113 A CN102251113 A CN 102251113A
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- vanadium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for purifying vanadium leaching solution and belongs to the technical field of purification of vanadium leaching solution after vanadium extraction from vanadium slag. The invention adopts a technical scheme that the method comprises: 1, setting the temperature of the leaching solution of a vanadium-containing clinker to be between 60 and 100 DEG C, and adding phosphorus-removing purifying agent; 2, regulating the pH value of vanadium leaching solution by using an acid and adding a silicon-removing purifying agent; and 3, after the reaction is finished, cooling, standing, and filtering to obtain vanadium solution with low silicon and phosphorus content. The method has the advantages that: the operation is simple, the requirements on the acidity and impurity content of original vanadium solution are low, the pH value after purification is 5 to 8, the reaction time and standing time of the vanadium solution are short, and the industrial and continuous production is made easier; and the whole purification system adopts sulfate, so the introduction of chlorine ions is avoided, environment pollution is avoided, equipment requirements are low, corrosion to a pipe in a subsequent process is relieved, and the treatment of acid waste water is promoted.
Description
Technical field
The present invention and a kind of method that leaches vanadium liquid purification and impurity removal belong to and leach vanadium liquid purification techniques field after the Leaching of Vanadium from Vanadium slag.
Background technology
Leaching of Vanadium from Vanadium slag takes the mode of oxidation sodium roasting to obtain grog mostly, leaches by intermittence or continous way and obtains containing vanadium solution, and in leaching process, impurity also enters in the vanadium liquid, as phosphorus, silicon, manganese, iron, aluminium, calcium, magnesium, sodium, chromium etc.Wherein be silicon and phosphorus to what precipitation and finished product had the greatest impact, the vanadium intermediates such as ammonium vanadate, the ammonium meta-vanadate etc. that are obtaining by removal of impurities liquid, silicon, phosphorus are difficult in the process of further deep processing and remove, directly have influence on the especially quality of vanadium iron of final finished, therefore need to carry out purification and impurity removal leaching vanadium liquid.At present, background technology mainly adopts the calcium chloride removal of impurities, and this method not only can dephosphorization, but also can remove the silicate ion of part solubility in the solution, and, because calcium chloride is ionogen, it can also destroy the suspended substance that has the electric double layer structure in the vanadium liquid, makes it to assemble sedimentation.But employing this method, the pH value that requires vanadium liquid are at 9-10, if surpass this scope, then cause a large amount of wastes of calcium chloride, and the silica removal rate is low, generates a large amount of vanadic acid calcium, cause vanadium to decrease, and in acid ammonium salt precipitation process, with the sulphur acid for adjusting pH value, also can generate a large amount of calcium sulfate, delay separating out of nucleus, reduce precipitation speed, influence the precipitation rate, gained ammonium vanadate grade is also lower, directly influences the quality of finished product.Publication number is that the Chinese invention patent application of CN101182036A discloses the technology that a kind of high vanadium removal of impurities prepares the high purity Vanadium Pentoxide in FLAKES, regulate desorbed solution pH8-9 with hydrochloric acid, employing Tai-Ace S 150 is scavenging agent, filtrate is used salt acid for adjusting pH value 8-9, under the situation of stirring at normal temperature, add ammonium chloride reaction 3-4 days, the centrifuge dehydration of the inclined to one side ammonium crystal of refining back gained, after the dehydration inclined to one side ammonium in the electro-forge stove at 500-550 ℃ of following calcination 6-8 hour, obtain the high purity Vanadium Pentoxide in FLAKES after the cooling.Publication number is that the Chinese invention patent application of CN101724757A discloses a kind of method of producing low-silicon and low-phosphorous vanadium liquid, the extraction temperature of vanadium bearing slag or the solvent temperature of thick vanadium product are arranged on 60 ℃ to the arbitrary temperature between the boiling, regulate above-mentioned vanadium liquid system with acid or alkali and be alkalescence, add scavenging agent and carry out silica removal, dephosphorization, scavenging agent is at least a in the group formed of aluminium salt, molysite, magnesium salts, question response finishes postcooling, filtration, obtains low-silicon and low-phosphorous vanadium liquid.The problem that above-mentioned two technology exist is: the technical scheme of CN101182036A only is confined to purify the purification of the vanadium liquid of navajoite after roasting, ion-exchange, does not relate to the vanadium slag grog and directly leaches the purification of complicated vanadium liquid of gained vanadium liquid composition; And scavenging solution pH value only limits to 8-9, and the reaction of vanadium liquid is longer, is unfavorable for industrial continuous production.The technical scheme removal of impurities of CN101724757A only is confined under the alkaline condition, if follow-up precipitation adopts the acid ammonium salt precipitation need strengthen the add-on of acid, has increased energy consumption.To sum up, the impurity removing technology of background technology all is confined under the alkaline condition for while dephosphorization, silica removal, and decontamination effect improving also has much room for improvement.
Summary of the invention
The object of the invention is to provide a kind of method that leaches vanadium liquid purification and impurity removal, scavenging solution pH value scope is wide, acid-basicity is less demanding, the purification efficiency height, remove phosphorus and silicon in the vanadium liquid targetedly respectively, obtain all lower vanadium liquid of silicon phosphorus content, lay a solid foundation, solve the problems referred to above that background technology exists for producing high-quality vanadium product.
Technical scheme of the present invention is as follows:
A kind of method that leaches vanadium liquid purification and impurity removal comprises following steps: 1. the temperature with vanadium-contained clinker leaching liquor is provided with between 60 ℃ to 100 ℃, adds the dephosphorization scavenging agent; 2. utilize acid to regulate the pH value that leaches vanadium liquid, add the silica removal scavenging agent; 3. after-filtration is cooled off, left standstill to above-mentioned reaction after finishing, and obtains the lower vanadium liquid of silicon phosphorus content.
Said vanadium-contained clinker leaching liquor can be for containing the leach liquor of the material after baking mixed such as vanadium raw materials and basic additive agent yellow soda ash, sodium-chlor, sodium sulfate, and this leaches vanadium liquid stoste pH value is 8-11.
Said dephosphorization scavenging agent is the mixed solution of ammonium sulfate and sal epsom, and the amount of sal epsom and ammonium sulfate is pressed mol ratio 1.0-2.0, the N of Mg and P and the mol ratio 1.0-2.0 of P adds.Said dephosphorization scavenging agent can add before leaching process, also can add in leaching vanadium liquid, and the reaction times is 10-20 minute.
The said pH value of utilizing sulfuric acid regulate to leach vanadium liquid is that the leaching stoste of 8-11 is adjusted to pH value 5-8 with the pH value.
Said desiliconizing agent is the aqueous solution of Tai-Ace S 150; The adding of desiliconizing agent Tai-Ace S 150 not only can be removed the element silicon in the vanadium liquid, also can further remove the phosphoric in the vanadium liquid; Adding the desiliconizing agent afterreaction time is 10-20 minute; The add-on of desiliconizing agent Tai-Ace S 150 is pressed alumina silica ratio 0.5-2.0 and is added.
Said cooling, leave standstill, the laboratory lab scale, time of repose is 1-3 hour, time of repose is 24-36 hour in the industrial production, just can obtain satisfying the low-silicon and low-phosphorous vanadium liquid of precipitation condition.
The invention has the beneficial effects as follows: simple to operate, less demanding to the acidity and the foreign matter content of original vanadium liquid, purify pH value 5-8, reaction of vanadium liquid and time of repose are all shorter, help industrial continuous production; The removal of impurities system all adopts vitriol, has avoided the introducing of chlorion, and environmental friendliness is low for equipment requirements, has reduced later process to Corrosion of Pipeline, helps the processing of acid waste water.
Description of drawings
Accompanying drawing 1 is schematic flow sheet of the present invention;
Embodiment:
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described by embodiment.
With reference to Fig. 1, a kind of method that leaches vanadium liquid purification and impurity removal comprises following steps: 1. the temperature with vanadium-contained clinker leaching liquor is provided with between 60 ℃ to 100 ℃, adds the dephosphorization scavenging agent; 2. utilize acid to regulate the pH value that leaches vanadium liquid, add the silica removal scavenging agent; 3. after-filtration is cooled off, left standstill to above-mentioned reaction after finishing, and obtains the lower vanadium liquid of silicon phosphorus content.
Said vanadium-contained clinker leaching liquor can be for containing the leach liquor of the material after baking mixed such as vanadium raw materials and basic additive agent yellow soda ash, sodium-chlor, sodium sulfate, and this leaches vanadium liquid stoste pH value is 8-11.
Said dephosphorization scavenging agent is the mixed solution of ammonium sulfate and sal epsom, and the amount of sal epsom and ammonium sulfate is pressed mol ratio 1.0-2.0, the N of Mg and P and the mol ratio 1.0-2.0 of P adds.Said dephosphorization scavenging agent can add before leaching process, also can add in leaching vanadium liquid, and the reaction times is 10-20 minute.
The said pH value of utilizing sulfuric acid regulate to leach vanadium liquid is that the leaching stoste of 8-11 is adjusted to pH value 5-8 with the pH value.
The sal epsom, ammonium sulfate, the Tai-Ace S 150 that add also can be their magnesium chloride, ammonium chloride, aluminum chloride, can also be magnesium nitrate, ammonium nitrate, aluminum nitrate, but consider environmental friendliness and decontamination effect improving, employing be sal epsom, ammonium sulfate, Tai-Ace S 150.
Said desiliconizing agent is the aqueous solution of Tai-Ace S 150; The adding of desiliconizing agent Tai-Ace S 150 not only can be removed the element silicon in the vanadium liquid, also can further remove the phosphoric in the vanadium liquid; Adding the desiliconizing agent afterreaction time is 10-20 minute; The add-on of desiliconizing agent Tai-Ace S 150 is pressed alumina silica ratio 0.5-2.0 and is added.
The chemical equation that the present invention relates to is as follows:
Mg
2++NH
4 ++PO
4 3-→?Mg(NH
4)PO
4?↓
Al
3++SiO
3 2-→?Al
2(SiO
3)
3↓。
Be the embodiment of laboratory of the present invention lab scale below.
Embodiment one
Present embodiment is taked dephosphorization in the vanadium slag grog leaching process, silica removal in the vanadium liquid.
In the clean beaker of 1000ml, add the grog that 400g obtains after by vanadium slag in the table 1 and additives roasting, and 80 ℃ of hot water of adding 800ml leach and stir, heating in water bath keeps this temperature, add 0.3g sal epsom, the solution that small amount of ammonium sulfate and suitable quantity of water were made into, stirred 10 minutes, stop heated and stirred, leave standstill suction filtration after for some time, filtrate is heated to 80 ℃, add the solution that 4.8g Tai-Ace S 150 and suitable quantity of water are made into, and to transfer pH with sulfuric acid be 8, react after 10 minutes, cooling was left standstill 60 minutes, filtration obtains [P]=5.65mg/L, the vanadium liquid of [Si]=264.31mg/L.
Embodiment two
Present embodiment is taked dephosphorization in the vanadium slag grog leaching process, silica removal in the vanadium liquid.
In the clean beaker of 1000ml, add the grog that 400g obtains after by vanadium slag in the table 1 and additives roasting, and 100 ℃ of hot water of adding 800ml leach and stir, heating in water bath, add 0.38g sal epsom, the solution that small amount of ammonium sulfate and suitable quantity of water were made into, stirred 15 minutes, stop heated and stirred, leave standstill suction filtration after for some time, filtrate is heated to 100 ℃, add the solution that 4.5g Tai-Ace S 150 and suitable quantity of water are made into, and to transfer pH with sulfuric acid be 6.5, react after 15 minutes, cooling was left standstill 100 minutes, filtration obtains [P]=4.60mg/L, the vanadium liquid of [Si]=230.89mg/L.
Certain vanadium slag main chemical compositions table/g.L-1 of table 1
Embodiment three
Present embodiment removes dephosphorization and silicon from the vanadium slag leach liquor.
Adding 800ml concentration in the clean beaker of 1000ml is 23.20g/L, phosphorus content 25.82mg/L, silicone content 432.38mg/L, the vanadium leachate of pH8.5 is heated to 60 ℃, adding 0.24g sal epsom, the solution that small amount of ammonium sulfate and suitable quantity of water were made into, stir after 5 minutes, add the solution that 8.6g Tai-Ace S 150 and suitable quantity of water are made into, and be 7.0, react after 10 minutes with sulfuric acid accent pH, stop heated and stirred, be cooled to room temperature, filter and obtain [P]=7.53mg/L, the vanadium liquid of [Si]=184.98mg/L.
Embodiment four
Present embodiment removes dephosphorization and silicon from the vanadium slag leach liquor.
Adding 800ml concentration in the clean beaker of 1000ml is 23.20g/L, phosphorus content 25.82mg/L, silicone content 432.38mg/L, the vanadium leachate of pH8.5 is heated to 80 ℃, adding 0.50g sal epsom, the solution that small amount of ammonium sulfate and suitable quantity of water were made into, stir after 10 minutes, add the solution that 5.8g Tai-Ace S 150 and suitable quantity of water are made into, and be 6.3, react after 8 minutes with sulfuric acid accent pH, stop heated and stirred, be cooled to room temperature, filter and obtain [P]=3.16mg/L, the vanadium liquid of [Si]=215.86mg/L.
Embodiment five
Present embodiment removes dephosphorization and silicon from the vanadium slag leach liquor.
Adding 800ml concentration in the clean beaker of 1000ml is 23.20g/L, phosphorus content 25.82mg/L, silicone content 432.38mg/L, the vanadium leachate of pH8.5 is heated to boiling, adding 0.40g sal epsom, the solution that small amount of ammonium sulfate and suitable quantity of water were made into, stir after 15 minutes, add the solution that 4.5g Tai-Ace S 150 and suitable quantity of water are made into, and be 7.5, react after 15 minutes with sulfuric acid accent pH, stop heated and stirred, be cooled to room temperature, filter and obtain [P]=5.24mg/L, the vanadium liquid of [Si]=209.08mg/L.
By above embodiment as can be seen, its phosphorus content of vanadium liquid that obtains according to the inventive method is all below 15mg/L, silicone content can be gone out the silicon phosphorus impurities in the vanadium leachate fast fast and effectively by present method below 300mg/L, can satisfy the requirement of industrial continuous production.
Claims (8)
1. method that leaches vanadium liquid purification and impurity removal, it is characterized in that comprising following steps: 1. the temperature with vanadium-contained clinker leaching liquor is provided with between 60 ℃ to 100 ℃, adds the dephosphorization scavenging agent; 2. utilize acid to regulate the pH value that leaches vanadium liquid, add the silica removal scavenging agent; 3. after-filtration is cooled off, left standstill to above-mentioned reaction after finishing, and obtains the lower vanadium liquid of silicon phosphorus content.
2. the method for leaching vanadium liquid purification and impurity removal according to claim 1, it is characterized in that said vanadium-contained clinker leaching liquor can be for containing the leach liquor of the material after baking mixed such as vanadium raw materials and basic additive agent yellow soda ash, sodium-chlor, sodium sulfate, this leaches vanadium liquid stoste pH value is 8-11.
3. the method for leaching vanadium liquid purification and impurity removal according to claim 1, it is characterized in that said dephosphorization scavenging agent is the mixed solution of ammonium sulfate and sal epsom, the amount of sal epsom and ammonium sulfate is pressed mol ratio 1.0-2.0, the N of Mg and P and the mol ratio 1.0-2.0 of P adds.
4. the method for leaching vanadium liquid purification and impurity removal according to claim 1 is characterized in that said dephosphorization scavenging agent can add before leaching process, also can add in leaching vanadium liquid, and the reaction times is 10-20 minute.
5. the method for leaching vanadium liquid purification and impurity removal according to claim 1 is characterized in that the said pH value of utilizing sulfuric acid regulate to leach vanadium liquid, is that the leaching stoste of 8-11 is adjusted to pH value 5-8 with the pH value.
6. the method for leaching vanadium liquid purification and impurity removal according to claim 1 is characterized in that said desiliconizing agent is the aqueous solution of Tai-Ace S 150.
7. the method for leaching vanadium liquid purification and impurity removal according to claim 1, it is characterized in that adding the desiliconizing agent afterreaction time is 10-20 minute; The add-on of desiliconizing agent Tai-Ace S 150 is pressed alumina silica ratio 0.5-2.0 and is added.
8. the method for leaching vanadium liquid purification and impurity removal according to claim 1 is characterized in that said cooling, leaves standstill, the laboratory lab scale, and time of repose is 1-3 hour, time of repose is 24-36 hour in the industrial production.
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Cited By (21)
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|---|---|---|---|---|
| CN102876899A (en) * | 2012-10-30 | 2013-01-16 | 重庆大学 | Method for effectively separating and extracting vanadium and chromium from vanadium-leaching wastewater |
| CN102943176A (en) * | 2012-11-08 | 2013-02-27 | 长沙矿冶研究院有限责任公司 | Method for removing silicon and phosphorus impurities from rich-vanadium desorption liquid |
| CN103409627A (en) * | 2013-07-09 | 2013-11-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing low-silicon low-calcium low-aluminium vanadium liquid |
| CN104046799A (en) * | 2013-12-03 | 2014-09-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Dephosphorization agent, and preparation method and application thereof |
| CN105132696A (en) * | 2015-09-10 | 2015-12-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium and removing phosphorus from high-calcium high-phosphorus vanadium slag |
| CN105331832A (en) * | 2015-11-27 | 2016-02-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Acid-leaching washing method for vanadium-containing roasting clinker |
| CN106521154A (en) * | 2016-12-01 | 2017-03-22 | 中信锦州金属股份有限公司 | Method for producing low-silicon chromic hydroxide by vanadium precipitation supernatant solution |
| CN106629846A (en) * | 2016-11-18 | 2017-05-10 | 河钢股份有限公司承德分公司 | Method for preparing ammonium polyvanadate from sodiumizing, roasting and leaching solution |
| CN108085517A (en) * | 2017-12-15 | 2018-05-29 | 河钢股份有限公司承德分公司 | A kind of preparation method of aerospace grade tablet vanadic anhydride |
| CN109161677A (en) * | 2018-09-28 | 2019-01-08 | 东北大学 | A method of vanadic anhydride is prepared using chromium type high vanadium slag |
| CN109234531A (en) * | 2018-10-23 | 2019-01-18 | 攀钢集团研究院有限公司 | Except the method for silicon phosphorus in alkaline solution containing vanadium |
| CN111052461A (en) * | 2017-09-15 | 2020-04-21 | 三樱工业株式会社 | Positive electrode active material, method for producing positive electrode active material, positive electrode, and secondary battery |
| CN111719053A (en) * | 2020-06-29 | 2020-09-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium and manganese by roasting vanadium slag |
| CN111778390A (en) * | 2020-07-08 | 2020-10-16 | 辽宁石化职业技术学院 | Purification method for producing vanadium pentoxide by sodium roasting |
| CN113481389A (en) * | 2021-06-02 | 2021-10-08 | 四川星明能源环保科技有限公司 | Method for removing phosphorus from vanadium-containing solution with high phosphorus content |
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| CN114315196A (en) * | 2021-11-23 | 2022-04-12 | 攀钢集团研究院有限公司 | Method for recovering silicon-phosphorus thermal insulation material from alkaline vanadium-containing liquid |
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| CN102876899A (en) * | 2012-10-30 | 2013-01-16 | 重庆大学 | Method for effectively separating and extracting vanadium and chromium from vanadium-leaching wastewater |
| CN102876899B (en) * | 2012-10-30 | 2013-09-11 | 重庆大学 | Method for effectively separating and extracting vanadium and chromium from vanadium-leaching wastewater |
| CN102943176A (en) * | 2012-11-08 | 2013-02-27 | 长沙矿冶研究院有限责任公司 | Method for removing silicon and phosphorus impurities from rich-vanadium desorption liquid |
| CN103409627A (en) * | 2013-07-09 | 2013-11-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing low-silicon low-calcium low-aluminium vanadium liquid |
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| CN105132696A (en) * | 2015-09-10 | 2015-12-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium and removing phosphorus from high-calcium high-phosphorus vanadium slag |
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| CN106521154A (en) * | 2016-12-01 | 2017-03-22 | 中信锦州金属股份有限公司 | Method for producing low-silicon chromic hydroxide by vanadium precipitation supernatant solution |
| CN111052461B (en) * | 2017-09-15 | 2023-10-10 | 三樱工业株式会社 | Positive electrode active material, method for producing positive electrode active material, positive electrode, and secondary battery |
| CN111052461A (en) * | 2017-09-15 | 2020-04-21 | 三樱工业株式会社 | Positive electrode active material, method for producing positive electrode active material, positive electrode, and secondary battery |
| CN108085517A (en) * | 2017-12-15 | 2018-05-29 | 河钢股份有限公司承德分公司 | A kind of preparation method of aerospace grade tablet vanadic anhydride |
| CN109161677A (en) * | 2018-09-28 | 2019-01-08 | 东北大学 | A method of vanadic anhydride is prepared using chromium type high vanadium slag |
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