CN103787414A - Method of preparing high-purity vanadium pentoxide from roasting-method vanadium solution - Google Patents
Method of preparing high-purity vanadium pentoxide from roasting-method vanadium solution Download PDFInfo
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- CN103787414A CN103787414A CN201410036279.9A CN201410036279A CN103787414A CN 103787414 A CN103787414 A CN 103787414A CN 201410036279 A CN201410036279 A CN 201410036279A CN 103787414 A CN103787414 A CN 103787414A
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- vanadium
- vanadium solution
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Abstract
The invention discloses a method of preparing high-purity vanadium pentoxide from roasting-method vanadium solution. The method comprises the following steps: adding a purifying agent into the roasting-method vanadium solution, wherein the purifying agent is polyaluminium chloride, magnesium chloride or calcium chloride, or the purifying agent is polyaluminium chloride and magnesium chloride, or polyaluminium chloride and calcium chloride; uniformly stirring the roasting-method vanadium solution containing the purifying agent, standing for settling, then filtering, and adding ammonium salt into the filtrate to precipitate vanadium; and finally, calcining meta-ammonium and deaminizing to prepare vanadium pentoxide with the purity being higher than 99.5%. Polyaluminium chloride serving as the purifying agent can be used for polymerizing jellies with several molecules into large particles with several tens of thousands of molecules, even hundreds of thousands of molecules. The large-particle molecular polymer is easy to settle in the vanadium solution and can be separated from the solution. The method provided by the invention has the advantages that the consumption of polyaluminium chloride is low, the flocculation process is simple, the flocculation capacity is strong, the flocculation speed is high, pollution is hardly caused and the cost is low.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of method of roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES.
Background technology
The method of high purity Vanadium Pentoxide in FLAKES is now all to dissolve and a series of scavenging process high purity Vanadium Pentoxide in FLAKES by ammonium meta-vanadate or ammonium poly-vanadate process.The production cost of this method is high, and environmental pollution is serious.With the doping roasting of scherbinaite colliery, low Ore Leaching, with strongly basic anionic resin exchange, desorb, 18 water Tai-Ace S 150 purify stripping liquid, stripping liquid adds ammonium salt precipitation after purifying, calcine to obtain Vanadium Pentoxide in FLAKES, this is the common production method of Vanadium Pentoxide in FLAKES, the Vanadium Pentoxide in FLAKES that the Vanadium Pentoxide in FLAKES that this production method can only production purity is 97% and purity are 98%, the highest can only production purity the Vanadium Pentoxide in FLAKES that is 99%.The impurity that in vanadium solution, the most difficult purification is removed is silica gel and aquation ironic hydroxide class jelly, phosphorus.First two material in vanadium solution mainly with several molecules or tens molecule (nH
2siO
3, mH
4siO
4, LNa
2siO
3, Fe (OH)
3nH
2o etc.) flock together, be present in vanadium solution with fine particle form, not sedimentation for a long time, by the method for common filtration, cannot separate these small particles, and phosphorus is to be also difficult to purify the impurity of removing.
Summary of the invention
The object of the invention is: a kind of method of roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES is provided, and its material consumption is few, and production process is simple, and environmental pollution is little, and production cost is low, and product purity is high, to overcome the deficiencies in the prior art.
The present invention is achieved in that the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, in roasting method vanadium solution, add scavenging agent, scavenging agent polymeric aluminum, magnesium chloride or calcium chloride, or polymeric aluminum and magnesium chloride or calcium chloride, after the roasting method vanadium solution that adds scavenging agent is stirred, staticly settle, filter, in filtrate, add ammonium salt to carry out precipitation, finally carry out inclined to one side ammonium calcining deamination and produce purity and reach more than 99.5% Vanadium Pentoxide in FLAKES.
When polymeric aluminum and calcium chloride use jointly, the add-on of polymeric aluminum is 1～2.5 times of silicon-dioxide quality in roasting method vanadium solution; The add-on of calcium chloride is 4～7.5 times of phosphorus quality in roasting method vanadium solution.
When polymeric aluminum and magnesium chloride use jointly, the add-on of polymeric aluminum is 2～7 times of silicon-dioxide quality in roasting method vanadium solution; The add-on of magnesium chloride is 1.5～5 times of phosphorus quality in roasting method vanadium solution.
Adding the roasting method vanadium solution of scavenging agent, is at 40～70 ℃ in temperature, stirs 15～35 minutes, filters after at room temperature staticly settling 70～75 hours.
Described roasting method vanadium solution is the vanadium solution of resin anion(R.A) exchange, desorb, and its pH value is 5～10.
Owing to having adopted technique scheme, compared with prior art, the present invention adopts polymeric aluminum as scavenging agent, and it can make the jelly of several molecules aggregate into tens thousand of, the even macrobead of tens0000 molecules.This oarse-grained Molecularly Imprinted Polymer just easily settles down in vanadium solution, opens with solution separating.Polymeric aluminum consumption of the present invention is little, and flocculation process is simple, and flocculation ability is strong, and flocculation rate is fast, pollutes littlely, and cost is low.If there is phosphorus to exist in vanadium solution, while purifying silica removal, polymeric aluminum and magnesium chloride or calcium chloride can together with add, add composite purifying agent, purify silica removal, iron and dephosphorization simultaneously.If there is no phosphorus in vanadium solution, or phosphorus content is little, as < 5mg/L, and can not dephosphorization, at this moment a polyaddition aluminium silica removal; And work as MgCl
2add-on be in vanadium solution when 3～6 times of phosphorus quality, after dephosphorization, in vanadium solution, the content of phosphorus drop to < 3mg/L, at this moment product V
2o
5in phosphorus content < 0.0003%.While purifying vanadium solution, can add separately polymeric aluminum silica removal and iron, add separately MgCl
2or CaCl
2dephosphorization also can add polymeric aluminum and MgCl simultaneously
2or polymeric aluminum and CaCl
2, composite purifying agent is removed silicon, iron and phosphorus.The present invention is simple and reliable, with low cost, and result of use is good.
Embodiment
Embodiments of the invention 1: the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, get 10 liters of stripping liquids, containing V
2o
515g/L, containing SiO
21.5g/L, containing Fe
2o
30.7 g/L, phosphorous 1g/L, its pH value is 10, takes 12 grams of polymeric aluminum, MgCl
240 grams, be dissolved in 1 premium on currency, heating vanadium solution to 40 ℃, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 30 minutes, and quiescent settling 70 hours under room temperature filters, and filtrate is containing SiO
20.008 g/L, containing Fe
2o
30.006g/L, phosphorous 0.0015 g/L, adds NH
4cl solution is (containing NH
4cl202.5 gram), precipitation, filtration, washing leaching cake calcining, obtain powdery V
2o
5146 grams.Detect its composition, containing SiO
20.065%, containing Fe
2o
30.006%, phosphorous 0.005%, in product Vanadium Pentoxide in FLAKES, the content of silicon, iron, phosphorus, respectively all lower than the content in high purity vanadic anhydride GB GB-3283-87 (issue on August 1st, 2010), reaches 99.5% V
2o
5.
Embodiments of the invention 2: the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, get 10 liters of stripping liquids, containing V
2o
530g/L, containing SiO
20.8g/L, containing Fe
2o
30.5g/L, phosphorous 0.6g/L, its pH value is 8.5; Take 20 grams of polymeric aluminum, MgCl
236 grams, be dissolved in 1 premium on currency, heating vanadium solution to 50 ℃, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 20 minutes, and quiescent settling 72 hours under room temperature filters; Filtrate is containing SiO
20.002g/L, phosphorous 0.0002g/L, containing Fe
2o
30.002g/L, adds NH
4cl solution is (containing NH
4cl405 gram), precipitation, filtration, washing leaching cake calcining, obtain powdery V
2o
5291.8 gram.Detect its composition, containing SiO
20.0075%, containing Fe
2o
30.004%, phosphorous 0.0028%, in product Vanadium Pentoxide in FLAKES, the content of silicon, iron, phosphorus, respectively all lower than the content in high purity vanadic anhydride GB GB-3283-87 (issue on August 1st, 2010), reaches 99.7% V
2o
5.
Embodiments of the invention 3: the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, get 10 liters of stripping liquids, containing V
2o
555g/L, containing SiO
20.75g/L, containing Fe
2o
30.6g/L, phosphorous 0.2g/L, its pH value is 5; Take 37 grams of polymeric aluminum, MgCl
215 grams, be dissolved in 1 premium on currency, heating vanadium solution to 60 ℃, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 15 minutes, and quiescent settling 73 hours under room temperature filters; Filtrate is containing SiO
20.0003g/L, containing Fe
2o
30.0001g/L, phosphorous 0.0001g/L, adds NH
4cl solution is (containing NH
4cl743 gram), precipitation, filtration, washing leaching cake calcining, obtain powdery V
2o
5534 grams.Detect its composition, containing SiO
20.002%, containing Fe
2o
30.0003%, phosphorous 0.0001 %, in product Vanadium Pentoxide in FLAKES, the content of silicon, iron, phosphorus, respectively all lower than the content in high purity vanadic anhydride GB GB-3283-87 (issue on August 1st, 2010), reaches 99.9% V
2o
5.
Embodiments of the invention 4: the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, get 10 liters of stripping liquids, containing V
2o
548g/L, containing SiO
20.5g/L, containing Fe
2o
30.35g/L, phosphorous 0.05g/L, its pH value is 7.5; Take 15 grams of polymeric aluminum, MgCl
25 grams, be dissolved in 1 premium on currency, heating vanadium solution to 70 ℃, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 15 minutes, and quiescent settling 70 hours under room temperature filters.Filtrate is containing SiO
20.006g/L, containing Fe
2o
30.004g/L, phosphorous 0.0001g/L, adds NH
4cl solution is (containing NH
4cl648 gram), precipitation, filtration, washing leaching cake calcining, obtain powdery V
2o
5463 grams.Detect its composition, containing SiO
20.0068%, containing Fe
2o
30.0035%, phosphorous 0.0001 %, in product Vanadium Pentoxide in FLAKES, the content of silicon, iron, phosphorus, respectively all lower than the content in high purity vanadic anhydride GB GB-3283-87 (issue on August 1st, 2010), reaches 99.7% V
2o
5.
Embodiments of the invention 5: the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, get 10 liters of stripping liquids, containing V
2o
543g/L, containing SiO
20.4g/L, containing Fe
2o
30.3g/L, phosphorous only have 0.002g/L, need not purify dephosphorization and just can reach the standard of high purity vanadic anhydride, and its pH value is 7; Take 18 grams of polymeric aluminum, be dissolved in 1 premium on currency, heating vanadium solution to 70 ℃, under agitation adds scavenging agent polymeric aluminum solution, stirs 15 minutes, and quiescent settling 72 hours under room temperature, filters.Filtrate is containing SiO
20.0004g/L, containing Fe
2o
30.0003g/L, phosphorous 0.002g/L, adds NH
4cl solution is (containing NH
4cl500 gram), precipitation, filtration, washing leaching cake calcining, obtain powdery V
2o
5416.6 gram.Detect its composition, containing SiO
20.0025%, containing Fe
2o
30.00035%, phosphorous 0.0025 %, in product Vanadium Pentoxide in FLAKES, the content of silicon, iron, phosphorus, respectively all lower than the content in high purity vanadic anhydride GB GB-3283-87 (issue on August 1st, 2010), reaches 99.9% V
2o
5.
Embodiments of the invention 6: the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, get 10 liters of stripping liquids, containing V
2o
538g/L, containing SiO
20.5g/L, containing Fe
2o
30.3g/L, phosphorous only have 0.3g/L, and its pH value is 9; Take 25 grams of polymeric aluminum, MgCl
28 grams, be dissolved in 1 premium on currency, heating vanadium solution to 70 ℃, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 15 minutes, and quiescent settling 70 hours under room temperature filters, and filtrate is containing SiO
20.00032g/L, containing Fe
2o
30.00015g/L, phosphorous 0.0008g/L, adds NH
4cl solution is (containing NH
4cl513 gram), precipitation, filtration, washing leaching cake calcining, obtain powdery V
2o
5368 grams.Detect its composition, containing SiO
20.0025%, containing Fe
2o
30.00036%, phosphorous 0.009%, in product Vanadium Pentoxide in FLAKES, the content of silicon, iron, phosphorus, respectively all lower than the content in high purity vanadic anhydride GB GB-3283-87 (issue on August 1st, 2010), reaches 99.5% V
2o
5.
Claims (5)
1. the method for a roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, it is characterized in that: in roasting method vanadium solution, add scavenging agent, scavenging agent polymeric aluminum, magnesium chloride or calcium chloride, or polymeric aluminum and magnesium chloride or calcium chloride, after the roasting method vanadium solution that adds scavenging agent is stirred, staticly settle, filter, in filtrate, add ammonium salt to carry out precipitation, finally carry out inclined to one side ammonium calcining deamination and produce purity and reach more than 99.5% Vanadium Pentoxide in FLAKES.
2. the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES according to claim 1, is characterized in that: the add-on of polymeric aluminum is 1～2.5 times of silicon-dioxide quality in roasting method vanadium solution; The add-on of calcium chloride is 4～7.5 times of phosphorus quality in roasting method vanadium solution.
3. the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES according to claim 1, is characterized in that: the add-on of polymeric aluminum is 2～7 times of silicon-dioxide quality in roasting method vanadium solution; The add-on of magnesium chloride is 1.5～5 times of phosphorus quality in roasting method vanadium solution.
4. the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES according to claim 1, it is characterized in that: the roasting method vanadium solution that adds scavenging agent, be at 40～70 ℃ in temperature, stir 15～35 minutes, filter after at room temperature staticly settling 70～75 hours.
5. the method for roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES according to claim 1, is characterized in that: described roasting method vanadium solution is the vanadium solution of resin anion(R.A) exchange, desorb, and its pH value is 5～10.
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Cited By (8)
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| CN104386747A (en) * | 2014-11-18 | 2015-03-04 | 河北钢铁股份有限公司承德分公司 | Method for preparing high-purity vanadium oxide employing ion exchange method |
| CN105087932A (en) * | 2015-09-01 | 2015-11-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing silicon in acid vanadium-enriched liquid and preparation method of vanadium oxide |
| US10053371B2 (en) | 2015-01-30 | 2018-08-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for preparing high-purity vanadium pentoxide powder |
| US10099939B2 (en) | 2015-01-30 | 2018-10-16 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium pentoxide powder |
| US10112846B2 (en) | 2015-01-30 | 2018-10-30 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium tetraoxide powder |
| US10125024B2 (en) | 2015-01-30 | 2018-11-13 | Institute Of Procees Engineering Chinese Academy Of Sciences | System and method for purifying and preparing high-purity vanadium pentoxide powder |
| CN109399712A (en) * | 2018-12-11 | 2019-03-01 | 联和能源投资控股有限公司 | A method of with hydrogen peroxide clean manufacturing high purity vanadic anhydride |
| US10294118B2 (en) | 2015-01-30 | 2019-05-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for purifying vanadium pentoxide |
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| CN104386747A (en) * | 2014-11-18 | 2015-03-04 | 河北钢铁股份有限公司承德分公司 | Method for preparing high-purity vanadium oxide employing ion exchange method |
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| US10125024B2 (en) | 2015-01-30 | 2018-11-13 | Institute Of Procees Engineering Chinese Academy Of Sciences | System and method for purifying and preparing high-purity vanadium pentoxide powder |
| US10294118B2 (en) | 2015-01-30 | 2019-05-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for purifying vanadium pentoxide |
| CN105087932A (en) * | 2015-09-01 | 2015-11-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing silicon in acid vanadium-enriched liquid and preparation method of vanadium oxide |
| CN105087932B (en) * | 2015-09-01 | 2017-08-25 | 攀钢集团攀枝花钢铁研究院有限公司 | The preparation method of the minimizing technology of silicon and vanadium oxide in rich acidic vanadium liquid |
| CN109399712A (en) * | 2018-12-11 | 2019-03-01 | 联和能源投资控股有限公司 | A method of with hydrogen peroxide clean manufacturing high purity vanadic anhydride |
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