CN103787414B - The method of roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES - Google Patents
The method of roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES Download PDFInfo
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- CN103787414B CN103787414B CN201410036279.9A CN201410036279A CN103787414B CN 103787414 B CN103787414 B CN 103787414B CN 201410036279 A CN201410036279 A CN 201410036279A CN 103787414 B CN103787414 B CN 103787414B
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Abstract
The invention discloses a kind of method of roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, scavenging agent is added in roasting method vanadium solution, scavenging agent polymeric aluminum, magnesium chloride or calcium chloride, or polymeric aluminum and magnesium chloride or calcium chloride, after the roasting method vanadium solution adding scavenging agent is stirred, staticly settle, filter, in filtrate, add ammonium salt carry out precipitation, finally carry out inclined ammonium calcining deamination and produce the Vanadium Pentoxide in FLAKES that purity reaches more than 99.5%.The present invention adopts polymeric aluminum as scavenging agent, and it can make the jelly of several molecule 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, and pollute little, 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 present high purity Vanadium Pentoxide in FLAKES is all pass through with ammonium meta-vanadate or ammonium poly-vanadate to dissolve and a series of scavenging process high purity Vanadium Pentoxide in FLAKES.The production cost of this method is high, and environmental pollution is serious.With the doping roasting of scherbinaite colliery, Weak-acid leaching, with strongly basic anionic resin exchange, desorb, 18 water Tai-Ace S 150 purification stripping liquids, ammonium salt precipitation is added after stripping liquid purification, calcine to obtain Vanadium Pentoxide in FLAKES, this is the general production method of Vanadium Pentoxide in FLAKES, this production method can only production purity be 97% Vanadium Pentoxide in FLAKES and purity be the Vanadium Pentoxide in FLAKES of 98%, the highest can only production purity be the Vanadium Pentoxide in FLAKES of 99%.In vanadium solution, the impurity of the most difficult purification removing is silica gel and aquation ironic hydroxide class jelly, phosphorus.First two material in vanadium solution mainly with several molecule 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 be separated the particle that these are small, phosphorus is also the impurity being difficult to purify removing.
Summary of the invention
The object of the invention is: a kind of method providing roasting method vanadium solution high purity Vanadium Pentoxide in FLAKES, 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, scavenging agent is added in roasting method vanadium solution, scavenging agent polymeric aluminum, magnesium chloride or calcium chloride, or polymeric aluminum and magnesium chloride or calcium chloride, after the roasting method vanadium solution adding scavenging agent is stirred, staticly settle, filter, in filtrate, add ammonium salt carry out precipitation, finally carry out inclined ammonium calcining deamination and produce the Vanadium Pentoxide in FLAKES that purity reaches more than 99.5%.
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.
Add the roasting method vanadium solution of scavenging agent, at temperature is 40 ~ 70 DEG C, stirs 15 ~ 35 minutes, filter after at room temperature staticly settling 70 ~ 75 hours.
Described roasting method vanadium solution is that resin anion(R.A) exchanges, the vanadium solution of desorb, and its pH value is 5 ~ 10.
Owing to have employed technique scheme, compared with prior art, the present invention adopts polymeric aluminum as scavenging agent, and it can make the jelly of several molecule 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, and pollute little, cost is low.If there is phosphorus to exist in vanadium solution, then when purifying silica removal, polymeric aluminum and magnesium chloride or calcium chloride can together with add, namely add composite purifying agent, purify silica removal, iron and dephosphorization simultaneously.If do not have 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 when being 3 ~ 6 times of phosphorus quality in vanadium solution, after dephosphorization, in vanadium solution, namely the content of phosphorus drop to < 3mg/L, at this moment product V
2o
5in phosphorus content < 0.0003%.Polymeric aluminum silica removal and iron can be added separately during purification vanadium solution, add MgCl separately
2or CaCl
2dephosphorization, also can add polymeric aluminum and MgCl simultaneously
2or polymeric aluminum and CaCl
2, i.e. composite purifying agent removing 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 stripping liquid 10 liters, containing V
2o
515g/L, containing SiO
21.5g/L, containing Fe
2o
30.7g/L, phosphorous 1g/L, its pH value is 10, takes polymeric aluminum 12 grams, MgCl
240 grams, be dissolved in 1 premium on currency, heating vanadium solution to 40 DEG C, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 30 minutes, standing at room temperature sedimentation 70 hours, filters, and filtrate is containing SiO
20.008g/L, containing Fe
2o
30.006g/L, phosphorous 0.0015g/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 is 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 stripping liquid 10 liters, 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 polymeric aluminum 20 grams, MgCl
236 grams, be dissolved in 1 premium on currency, heating vanadium solution to 50 DEG C, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 20 minutes, standing at room temperature sedimentation 72 hours, 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 is 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 stripping liquid 10 liters, 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 polymeric aluminum 37 grams, MgCl
215 grams, be dissolved in 1 premium on currency, heating vanadium solution to 60 DEG C, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 15 minutes, standing at room temperature sedimentation 73 hours, 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 is 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 stripping liquid 10 liters, 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 polymeric aluminum 15 grams, MgCl
25 grams, be dissolved in 1 premium on currency, heating vanadium solution to 70 DEG C, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 15 minutes, standing at room temperature sedimentation 70 hours, 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 is 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 stripping liquid 10 liters, containing V
2o
543g/L, containing SiO
20.4g/L, containing Fe
2o
30.3g/L, phosphorous only have 0.002g/L, and need not purify the standard that dephosphorization just can reach high purity vanadic anhydride, its pH value is 7; Take polymeric aluminum 18 grams, be dissolved in 1 premium on currency, heating vanadium solution to 70 DEG C, under agitation adds scavenging agent polymeric aluminum solution, stirs 15 minutes, standing at room temperature sedimentation 72 hours, 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 is 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 stripping liquid 10 liters, 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 polymeric aluminum 25 grams, MgCl
28 grams, be dissolved in 1 premium on currency, heating vanadium solution to 70 DEG C, under agitation adds scavenging agent polymeric aluminum and MgCl
2solution, stirs 15 minutes, standing at room temperature sedimentation 70 hours, 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 is 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 is polymeric aluminum or polymeric aluminum and magnesium chloride or polymeric aluminum and calcium chloride, after the roasting method vanadium solution adding scavenging agent is stirred, staticly settle, filter, in filtrate, add ammonium salt carry out precipitation, finally carry out inclined ammonium calcining deamination and produce the Vanadium Pentoxide in FLAKES that purity reaches more than 99.5%.
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 adding scavenging agent, at temperature is 40 ~ 70 DEG C, stirs 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 that resin anion(R.A) exchanges, the vanadium solution of desorb, and its pH value is 5 ~ 10.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104386747B (en) * | 2014-11-18 | 2016-03-30 | 河北钢铁股份有限公司承德分公司 | A kind of ion exchange method prepares the method for high purity barium oxide |
| CN105984900B (en) | 2015-01-30 | 2017-06-13 | 中国科学院过程工程研究所 | A kind of system and method for preparing high purity vanadic anhydride powder |
| CN105984899B (en) | 2015-01-30 | 2017-05-17 | 中国科学院过程工程研究所 | System and method for purifying vanadium pentoxide |
| CN105984897B (en) | 2015-01-30 | 2017-05-17 | 中国科学院过程工程研究所 | System and method for producing high-purity vanadium pentoxide powder |
| CN105984898B (en) | 2015-01-30 | 2017-06-13 | 中国科学院过程工程研究所 | A kind of system and method for producing high-purity vanadium tetraoxide powder |
| CN105984896B (en) | 2015-01-30 | 2017-06-13 | 中国科学院过程工程研究所 | A kind of purification prepares the system and method for high purity vanadic anhydride powder |
| 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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| US20050165132A1 (en) * | 2004-01-28 | 2005-07-28 | Xerox Corporation | Toner processes |
| CN101759313A (en) * | 2009-12-08 | 2010-06-30 | 武汉科技大学 | Method for recycling high-salinity heavy metal-enriched waste water from vanadium extraction from stone coal |
| CN102864318A (en) * | 2012-10-16 | 2013-01-09 | 长沙矿冶研究院有限责任公司 | Method for recycling vanadium from acid vanadium-containing solution containing silicon and phosphorus |
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2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050165132A1 (en) * | 2004-01-28 | 2005-07-28 | Xerox Corporation | Toner processes |
| CN101759313A (en) * | 2009-12-08 | 2010-06-30 | 武汉科技大学 | Method for recycling high-salinity heavy metal-enriched waste water from vanadium extraction from stone coal |
| CN102864318A (en) * | 2012-10-16 | 2013-01-09 | 长沙矿冶研究院有限责任公司 | Method for recycling vanadium from acid vanadium-containing solution containing silicon and phosphorus |
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