CN101157478A - Preparation method of ammonium poly-vanadate - Google Patents

Preparation method of ammonium poly-vanadate Download PDF

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Publication number
CN101157478A
CN101157478A CNA2007102017543A CN200710201754A CN101157478A CN 101157478 A CN101157478 A CN 101157478A CN A2007102017543 A CNA2007102017543 A CN A2007102017543A CN 200710201754 A CN200710201754 A CN 200710201754A CN 101157478 A CN101157478 A CN 101157478A
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vanadium
solution
calcium
value
vanadate
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CNA2007102017543A
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Chinese (zh)
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CN100558643C (en
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彭毅
李千文
夏清荣
王小江
彭明福
付自碧
窦伟
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攀钢集团攀枝花钢铁研究院
攀枝花新钢钒股份有限公司
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Priority to CNB2007102017543A priority Critical patent/CN100558643C/en
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Abstract

The invention belongs to the chemical engineering field, in particular relates to a method for preparing ammonium polyvandata with vanadium-containing solution. The method uses the vanadium-containing solution produced with the traditional sodium roasting-water immersing technology as the raw material. First, vanadium combines with added calcium compounds and produces calcium vanadate, which reacts with ammonium bicarbonate and transfers vanadium into the solution but transforms calcium into more insoluble calcium carbonate; the ammonium polyvandata is produced with the separated solution under appropriate pH and heating conditions. After redissolution of calcium vandata, the ammonium bicarbonate containing less than 0.1percent of SUM (Na2O+K2 O) can be obtained. The ammonium bicarbonate can be used for production of vanadium trioxide and vanadium pentoxide with exceedingly low contents of potassium and sodium; and the ammonia content of vanadium-precipitation waste water is only 60percent to 75 percent of vanadium-extraction waste water in traditional technologies. The invention has very promising application prospect.

Description

A kind of preparation method of ammonium poly-vanadate
Technical field
The invention belongs to chemical field, be specifically related to a kind of usefulness and contain the method that vanadium solution is produced ammonium poly-vanadate.
Background technology
Vanadium is the high-melting-point rare metal, has a lot of good performances, has been widely used in industries such as metallurgy, chemical industry.Along with the high speed development of China's modernization construction, the demand of vanadium and compound thereof is increasing, and use range is more and more wider, and its specification of quality is also higher.In the VN alloy production process, require the ∑ (Na in the vanadium oxide raw material 2O+K 2O) content is low more good more, and in the vanadium oxide product that traditional sodium roasting-the water law process for extracting vanadium is produced, ∑ (Na 2O+K 2O) content is higher than VN alloy far away to raw material ∑ (Na generally 0.5%~2% 2O+K 2O) requirement of content has very big influence to production cost, production unit and the production environment of VN alloy, and the life-span that makes the VN alloy production unit is only by about 100 days.In addition, with ammonia content is up to 4~10g/L in the waste water that is produced in traditional sodium roasting-water law process for extracting vanadium production vanadium oxide process, environmental pollution is serious, is difficult to administer, and also can't recycle.
Be published in " vanadium titanium " document of the 3rd phase of nineteen ninety " from industrial Vanadium Pentoxide in FLAKES, extracting vanadic acid calcium " and introduced a kind of method of producing vanadic acid calcium, its method is the basic solution that is configured to vanadic acid sodium with analytical pure, adds the calcium chloride solution reaction then and promptly gets the vanadic acid calcium product.The document only illustrates with sodium vanadate solution and calcium chloride reaction can obtain vanadic acid calcium, does not introduce the vanadic acid calcium method of producing ammonium poly-vanadate.
Be published in " Henan chemical industry " document of the 1st phase in 1999 " soaking the technical study that reclaims vanadium the solution from containing vanadic acid " and introduced a kind of method that reclaims vanadium from acid dip solution, its method is precipitation vanadic acid calcium-carbonating leaching-precipitation ammonium poly-vanadate.The document has been introduced processing parameters such as temperature of reaction that precipitation vanadic acid calcium and carbonating leach, time, pH value, is the very low solution of vanadium concentration but test usefulness contains the vanadic acid immersion liquid; When carbonating leached, the add-on of volatile salt was very big, finally causes production cost big, and the ammonia content in the vanadium wastewater is very high; Whole technology vanadium total recovery only is about 90%, and the potassium sodium content fails to carry out control corresponding in the ammonium poly-vanadate product.
This area need be developed a kind of preparation method of ammonium poly-vanadate of low potassium sodium content at present.
Summary of the invention
The objective of the invention is to overcome above shortcoming, provide a kind of potassium sodium content low ammonium poly-vanadate preparation method.The vanadium oxide product of the ammonium poly-vanadate production of producing with this technology has the low characteristics of potassium sodium content, and the ammonia content in the vanadium wastewater also only is 60%~75% of a traditional technology.
In conjunction with purpose of the present invention, realize by following technical solution:
A kind of preparation method of ammonium poly-vanadate may further comprise the steps:
A, in containing vanadium leachate, add calcium salt soln;
B, the vanadium solution that contains that will add calcium salt are regulated pH value to alkaline;
C, with system heating, stir, the vanadic acid calcium deposit, refilter, wash;
D, will filter vanadic acid calcium join in the solution that contains leaching agent, solution is heated the certain hour after-filtration;
E, filtrate is regulated pH value to 1.8~2.5,90 ℃ to the boiling condition, stirring 40min~60min precipitation obtains ammonium poly-vanadate after the filtration.
Wherein, the full content of vanadium that contains vanadium leachate among the aforesaid method step a is 10~60g/L.
Wherein, the calcium salt among the aforesaid method step a is calcium chloride or nitrocalcite, and add-on is pressed V: Ca=1: 1.2~2 quality ratio is determined.
Wherein, regulating the pH value among the aforesaid method step b is to adopt lime milk solution to carry out.
Wherein, the solution system pH value when precipitating vanadic acid calcium among the aforesaid method step c is 8.5~10, and the temperature of heating is 80 ℃ of extremely boilings, and the reaction times is 30min~60min.Longer with the time when system temperature is 80 ℃, as it is shorter to be heated to the then used time of boiling.
Wherein, the leaching agent in the aforesaid method steps d is a bicarbonate of ammonia, and the add-on of bicarbonate of ammonia is worth in molar ratio counts CO 3 2-: Ca 2+=1: 1~1.5.General operating weight concentration is 5%~15% ammonium bicarbonate soln.
Wherein, vanadic acid calcium decalcification leaching temperature of reaction is 50 ℃ of extremely boilings in the aforesaid method steps d, and the leaching reaction times is 30min~70min.Longer with the time when system temperature is 50 ℃, shorter as system for the then used time of boiling.
Wherein, the reagent of adjusting filtrate pH value is sulfuric acid among the aforesaid method step e.
The beneficial effect of the inventive method is: compare with direct precipitation ammonium poly-vanadate technology, the inventive method can use directly that the vanadium leachate that contains of gained is starting raw material in the existing production, and obtain Na in the ammonium poly-vanadate product 2O+K 2O content is more much lower than the ammonium poly-vanadate that obtains with existing method, this product especially is suitable as raw materials for production production VN alloy, can significantly reduce corrosion to the VN alloy production unit, the life-span of VN alloy production unit can be brought up to more than 1 year by original about about 100 days, can also the vanadium-nitrogen alloy product quality also obviously improve simultaneously.In addition, the vanadium grade of the ammonium poly-vanadate of gained greatly improves, and therefore can directly apply to the production process of vanadium product, and can also reduce the ammonia concentration in the waste water greatly, can bring good economic benefits and social benefit, has good application prospects.
Description of drawings
What Fig. 1 represented is the concise and to the point flow process of the inventive method
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment one usefulness the inventive method prepares ammonium poly-vanadate
Getting vanadium concentration is the solution 1400ml of 33.1g/L, adds the calcium chloride solution 188ml of 500g/L; Under stirring condition, adding milk of lime regulator solution pH value is 9.46; Be heated to boiling reaction 40min.Obtain vanadic acid calcium 153.1g, vanadic acid calcium TV is 29.83%; Precipitation vanadic acid calcium supernatant liquor volume is 1120ml, and TV is 0.408g/L; Vanadic acid calcium washings volume is 267ml, and TV is 0.128g/L; The vanadium deposition rate is 98.94%.
Get this vanadic acid calcium 100g that contains vanadium 29.83%, join 1000ml and contain in the solution of bicarbonate of ammonia 5%, be heated with stirring to boiling, reaction 30min.After-filtration is finished in reaction, washes precipitation with water, and filtrate and wash water merge, and volume is 1440mL, and TV content is 20.25g/L, and the vanadium leaching yield is 97.77%.Leach liquor is regulated the back precipitation of pH value, and gained ammonium poly-vanadate main component is behind the filtration washing: TV=49.20%, Ca=0.45%, Fe<0.01%, Si=0.05%, S=0.412%, K<0.005%, Na=0.009%; Precipitation supernatant liquor and washing water merge NH in the gained vanadium wastewater of back 3=3.46g/L.
Embodiment dual-purpose the inventive method prepares ammonium poly-vanadate
Getting vanadium concentration is the solution 1000ml of 51.82g/L, adds the calcium chloride solution 210ml of 500g/L; Under stirring condition, adding milk of lime regulator solution pH value is 9.26; Be heated to boiling, reaction 30min.Obtain vanadic acid calcium 185.2g, vanadic acid calcium TV is 27.62%; Precipitation vanadic acid calcium supernatant liquor volume is 990ml, and TV is 0.58g/L; Vanadic acid calcium washings volume is 210ml, and TV is 0.054g/L; The vanadium deposition rate is 98.87%.
Get this vanadic acid calcium 100g that contains vanadium 27.62%, join 350mL and contain in the solution of bicarbonate of ammonia 15%, be heated with stirring to boiling, reaction 30min.After-filtration is finished in reaction, washes precipitation with water, and solution and wash water merge, and volume is 825mL, and TV content is 32.82g/L, and the vanadium leaching yield is 98.03%.Leach liquor is regulated the back precipitation of pH value, and gained ammonium poly-vanadate main component is behind the filtration washing: TV=49.40%, Ca=0.55%, Fe<0.01%, Si=0.06%, S=0.430%, K<0.005%, Na=0.008%; Precipitation supernatant liquor and washing water merge NH in the gained vanadium wastewater of back 3=3.92g/L.
Embodiment three usefulness the inventive method prepare ammonium poly-vanadate
Getting vanadium concentration is the solution 1000ml of 35.6g/L, adds the ca nitrate soln 200ml of 500g/L; Under stirring condition, adding milk of lime regulator solution pH value is 9.1; Be heated to boiling, reaction 30min.Obtain vanadic acid calcium 107.98g, vanadic acid calcium TV is 32.45%; After precipitation vanadic acid calcium supernatant liquor and wash water merged, volume was 1550ml, and TV is 0.36g/L, and the vanadium deposition rate is 98.43%.
Get this vanadic acid calcium 100g that contains vanadium 32.45%, join 350mL and contain in the solution of bicarbonate of ammonia 15%, be heated with stirring to 85 ℃, reaction 60min.After-filtration is finished in reaction, washs precipitation with less water, and solution and wash water merge, and volume is 886mL, and TV content is 36.2g/L, and the vanadium leaching yield is 98.82%.Leach liquor is regulated the back precipitation of pH value, and gained ammonium poly-vanadate main component is behind the filtration washing: TV=50.16%, Ca=0.31%, Fe<0.01%, Si=0.04%, S=0.04%, K<0.005%, Na=0.007%; Precipitation supernatant liquor and washing water merge NH in the gained vanadium wastewater of back 3=3.47g/L.
Therefore the inventive method uses directly that the vanadium leachate that contains of gained is starting raw material in the existing production, and obtain Na in the ammonium poly-vanadate product 2O+K 2O content is more much lower than the ammonium poly-vanadate that obtains with existing method, the ammonium poly-vanadate production VN alloy of using the inventive method to make in the actual production, significantly reduced corrosion to the VN alloy production unit, make the VN alloy production unit by before normal use of intensity still can also continue in 1 year to use, can also the vanadium-nitrogen alloy product quality also be significantly improved simultaneously.In addition, the ammonia concentration in the waste water that the inventive method produced also reduces greatly, brings good economic benefits and social benefit, has good application prospects.

Claims (8)

1. the preparation method of an ammonium poly-vanadate is characterized in that may further comprise the steps:
A, in containing vanadium leachate, add calcium salt soln;
B, the vanadium solution that contains that will add calcium salt are regulated pH value to alkaline;
C, with system heating, stir, the vanadic acid calcium deposit, refilter, wash;
D, will filter vanadic acid calcium join in the solution that contains leaching agent, solution is heated the certain hour after-filtration;
E, filtrate is regulated pH value to 1.8~2.5,90 ℃ to the boiling condition, stirring 40min~60min precipitation obtains ammonium poly-vanadate after the filtration.
2. method according to claim 1 is characterized in that: the described full content of vanadium that contains vanadium leachate is 10~60g/L.
3. method according to claim 1 is characterized in that: the calcium salt described in the step a is calcium chloride or nitrocalcite, and add-on is pressed V: Ca=1: the quality ratio of (1.2~2) is determined.
4. method according to claim 1 is characterized in that: the adjusting pH value described in the step b adopts lime milk solution to carry out.
5. method according to claim 1 is characterized in that: the pH value of solution value the during vanadic acid of precipitation described in step c calcium is 8.5~10, and the temperature of heating is 80 ℃ of extremely boilings, and the reaction times is 30min~60min.
6. method according to claim 1 is characterized in that: the leaching agent described in the steps d is a bicarbonate of ammonia, and the add-on of bicarbonate of ammonia is worth in molar ratio counts CO 3 2-: Ca 2+=1: (1~1.5).
7. method according to claim 1 is characterized in that: it is 50 ℃ of extremely boilings that temperature of reaction is leached in the vanadic acid calcium decalcification described in the steps d, and the leaching reaction times is 30min~70min.
8. method according to claim 1 is characterized in that: the reagent of regulating filtrate pH value among the step e is sulfuric acid.
CNB2007102017543A 2007-09-18 2007-09-18 A kind of preparation method of ammonium poly-vanadate CN100558643C (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010057410A1 (en) * 2008-11-18 2010-05-27 Panzhihua New Steel & Vanadium Co., Ltd. Clean production method of vanadium oxide
WO2010057411A1 (en) * 2008-11-18 2010-05-27 Panzhihua New Steel & Vanadium Co., Ltd. Production method of vanadium oxide using ion-exchange to realize wastewater circulation
CN102050491A (en) * 2010-11-29 2011-05-11 中信锦州金属股份有限公司 Vanadium trioxide production method
CN102328954A (en) * 2011-08-04 2012-01-25 佛山市邦普循环科技有限公司 Method for recovering vanadium from lithium vanadium phosphate power battery for electric automobile
CN102476829A (en) * 2010-11-30 2012-05-30 攀钢集团钢铁钒钛股份有限公司 Preparation method of vanadyl sulfate
CN102534233A (en) * 2012-02-10 2012-07-04 四川省达州钢铁集团有限责任公司 Vanadium extraction technology of low-grade high-calcium vanadium-containing steel slag
CN102758088A (en) * 2012-06-07 2012-10-31 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing high-density ammonium poly-vanadate and wet vanadium extracting process
CN102912130A (en) * 2012-11-13 2013-02-06 吉首大学 Method for separating vanadium enriched in stone coal leaching solution
CN102994751A (en) * 2011-09-13 2013-03-27 攀钢集团攀枝花钢铁研究院有限公司 Method for reducing concentration of calcium ions in calcium-containing solution
CN104538660A (en) * 2014-12-25 2015-04-22 河北钢铁股份有限公司承德分公司 Preparation method of high-purity vanadium oxide suitable for all-vanadium flow battery
CN104843789A (en) * 2015-04-30 2015-08-19 河北钢铁股份有限公司承德分公司 Method for purifying vanadium pentoxide
CN106164304A (en) * 2014-03-11 2016-11-23 韩国地质资源研究院 Vanadium and the method for tungsten is reclaimed from the leachate of denitration waste catalyst
CN107937737A (en) * 2017-11-24 2018-04-20 攀钢集团攀枝花钢铁研究院有限公司 A kind of method for reducing chromium content in high chromium calcium vanadate
CN107964601A (en) * 2017-11-24 2018-04-27 攀钢集团攀枝花钢铁研究院有限公司 A kind of method of chromium content in reduction calcium vanadate

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* Cited by examiner, † Cited by third party
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GB1269639A (en) * 1968-07-12 1972-04-06 Murex Ltd Preparation of sodium ammonium polyvanadate and ammonium metavanadate
IT1196514B (en) * 1986-07-17 1988-11-16 Ente Minerario Siciliano Process for recovering vanadium from residues from the combustion of petroleum fractions
CN1059885A (en) * 1990-07-24 1992-04-01 湖南省煤炭科学研究所 A kind of novel method of from contain the scherbinaite coal, extracting Vanadium Pentoxide in FLAKES
CN1207409C (en) * 2003-05-08 2005-06-22 锦州铁合金(集团)有限责任公司 Wet process of extracting vanadium and/or molybdenum from waste catalyst

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010057410A1 (en) * 2008-11-18 2010-05-27 Panzhihua New Steel & Vanadium Co., Ltd. Clean production method of vanadium oxide
WO2010057411A1 (en) * 2008-11-18 2010-05-27 Panzhihua New Steel & Vanadium Co., Ltd. Production method of vanadium oxide using ion-exchange to realize wastewater circulation
RU2454368C1 (en) * 2008-11-18 2012-06-27 Панган Груп Стил Ванадиум & Титаниум Ко., Лтд. Method of producing vanadium oxide using ion exchange to recycle waste water
CN102050491A (en) * 2010-11-29 2011-05-11 中信锦州金属股份有限公司 Vanadium trioxide production method
CN102050491B (en) * 2010-11-29 2012-04-18 中信锦州金属股份有限公司 Vanadium trioxide production method
CN102476829B (en) * 2010-11-30 2013-06-12 攀钢集团钢铁钒钛股份有限公司 Preparation method of vanadyl sulfate
CN102476829A (en) * 2010-11-30 2012-05-30 攀钢集团钢铁钒钛股份有限公司 Preparation method of vanadyl sulfate
CN102328954B (en) * 2011-08-04 2013-06-26 佛山市邦普循环科技有限公司 Method for recovering vanadium from lithium vanadium phosphate power battery for electric automobile
CN102328954A (en) * 2011-08-04 2012-01-25 佛山市邦普循环科技有限公司 Method for recovering vanadium from lithium vanadium phosphate power battery for electric automobile
CN102994751B (en) * 2011-09-13 2014-10-01 攀钢集团攀枝花钢铁研究院有限公司 Method for reducing concentration of calcium ions in calcium-containing solution
CN102994751A (en) * 2011-09-13 2013-03-27 攀钢集团攀枝花钢铁研究院有限公司 Method for reducing concentration of calcium ions in calcium-containing solution
CN102534233A (en) * 2012-02-10 2012-07-04 四川省达州钢铁集团有限责任公司 Vanadium extraction technology of low-grade high-calcium vanadium-containing steel slag
CN102758088A (en) * 2012-06-07 2012-10-31 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing high-density ammonium poly-vanadate and wet vanadium extracting process
CN102912130A (en) * 2012-11-13 2013-02-06 吉首大学 Method for separating vanadium enriched in stone coal leaching solution
CN106164304A (en) * 2014-03-11 2016-11-23 韩国地质资源研究院 Vanadium and the method for tungsten is reclaimed from the leachate of denitration waste catalyst
CN104538660A (en) * 2014-12-25 2015-04-22 河北钢铁股份有限公司承德分公司 Preparation method of high-purity vanadium oxide suitable for all-vanadium flow battery
CN104843789A (en) * 2015-04-30 2015-08-19 河北钢铁股份有限公司承德分公司 Method for purifying vanadium pentoxide
CN107937737A (en) * 2017-11-24 2018-04-20 攀钢集团攀枝花钢铁研究院有限公司 A kind of method for reducing chromium content in high chromium calcium vanadate
CN107964601A (en) * 2017-11-24 2018-04-27 攀钢集团攀枝花钢铁研究院有限公司 A kind of method of chromium content in reduction calcium vanadate
CN107964601B (en) * 2017-11-24 2019-06-14 攀钢集团攀枝花钢铁研究院有限公司 A kind of method of chromium content in reduction calcium vanadate

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