CN1294084C - Method of preparing high density ammonium polyvanadate - Google Patents
Method of preparing high density ammonium polyvanadate Download PDFInfo
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- CN1294084C CN1294084C CNB2004100400123A CN200410040012A CN1294084C CN 1294084 C CN1294084 C CN 1294084C CN B2004100400123 A CNB2004100400123 A CN B2004100400123A CN 200410040012 A CN200410040012 A CN 200410040012A CN 1294084 C CN1294084 C CN 1294084C
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- vanadium
- vanadate
- sulfuric acid
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- ammonium poly
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Abstract
The present invention provides a preparation method for high-density ammonium polyorthovanadate precipitated and prepared from ammonia water, which has the advantages of safety, convenience and no generation of irritant smell. The preparation method comprises the following steps: 1), sulfuric acid is added in a vanadium containing solution to regulate a pH value; 2), the sulfuric acid and the ammonia water which need to be added are equally divided into at least three equal parts and are added to the vanadium containing solution by at least three steps in an order that the sulfuric acid is added firstly and the ammonia water is added subsequently; 3), the sulfuric acid is added to regulate the pH value of the solution; 4), active ammonium polyorthovanadate crystal seeds are added, and the high-density ammonium polyorthovanadate obtained by filtration, washing and drying after a temperature is increased and vanadium is precipitated. Since the synthesis of ammonium sulfate is carried out in a vanadium precipitating tank, the sulfuric acid used for neutralizing the ammonia water is firstly added in the vanadium precipitating tank by batches, the ammonia water is subsequently added in the vanadium precipitating tank by the batches and the pH value of the solution is ensured to be less than 7 in the whole process of ammonification, no irritant smell is generated in an operation process, which is favorable for the physical health of operators.
Description
Technical field
The invention belongs to chemical industry, metallurgical technology field, relate in particular to a kind of ammoniacal liquor of using, prepare the method for high-density ammonium poly-vanadate as precipitation agent.
Background technology
The existing method of producing ammonium poly-vanadate from contain vanadium solution is under acidic conditions, as precipitation agent, is settled out ammonium poly-vanadate with ammonium salt (as ammonium sulfate, ammonium nitrate or volatile salt etc.) under the boiling condition, produces V through subsequent handling again
2O
5Or V
2O
3Choosing which kind of ammonium salt, to make precipitation agent closely related with desired ammonium poly-vanadate quality of follow-up vanadium product and production cost.For producing the V that is used for the vanadium iron raw material
2O
3The desired high-density ammonium poly-vanadate of product requires the density of ammonium poly-vanadate to be not less than 0.6g/cm
3Having described a kind of among the CN98124042.9 is that precipitation agent is produced the high-density ammonium poly-vanadate with ammonium sulfate.Produce the high-density ammonium poly-vanadate with ammonium sulfate as precipitation agent, exist the production cost height, the shortcoming that labour intensity is big.
" from spent vanadium catalyst, the reclaiming vanadium " of delivering on " directly acidleach contains the technical study of vanadium lime-ash vanadium extraction " that Tangshan Engineering College journal (91. (2) .75-80) is delivered and U.S. Pat 4788044 " Recovering vanadium frompetroleum fraction combustion residue " and the chemistry world (1991.32 (5)) with solvent extration, in these three parts of data, ammoniacal liquor is used as a kind of good ammonium poly-vanadate precipitation agent.Compare with other ammonium salt, ammoniacal liquor has very big advantage economically, can reduce the production cost of vanadium greatly, improves the market competitiveness of enterprise significantly.But produce ammonium poly-vanadate with ammoniacal liquor as precipitation agent, exist bigger irritating smell, the shortcoming of work under bad environment is produced the high-density ammonium poly-vanadate and is difficult to control condition especially.
Summary of the invention
Technical problem to be solved by this invention provide a kind of safe, convenient have no irritating odor again produce produce the preparation method of high-density ammonium poly-vanadate with ammonia precipitation process.
The technical scheme that technical solution problem of the present invention is adopted is: a kind of method for preparing the high-density ammonium poly-vanadate, may further comprise the steps: 1) will contain vanadium solution, adding the sulphur acid for adjusting pH value is 2.5～5.0,2) sulfuric acid that will add and ammoniacal liquor are divided into trisection at least, earlier sulfuric acid being divided into at least three steps joins and contains in the vanadium solution, and then ammoniacal liquor was divided into at least three steps joins and contain in the vanadium solution, 3) the pH value 1.8～2.5 of adding sulfuric acid regulation solution, 4) add active ammonium poly-vanadate crystal seed, after the intensification precipitation, filter, after the washing, oven dry promptly.
Above-mentioned steps 1) concentration that contains vanadium in the vanadium solution in is 20～40g/l.The temperature that contains vanadium solution in the step 1) is 70 ℃～90 ℃.Described sulfuric acid concentration is 96%～98%.Described step 2) NH of ammoniacal liquor in
3Concentration is 18%～30%.The add-on of described sulfuric acid and ammoniacal liquor is calculated by following formula:
NH wherein
3/ V=0.5～0.65.PH value in the described step 1) is 2.5～5.0, and the pH value in the step 3) is 1.8～2.5.Total vanadium amount of the active ammonium poly-vanadate crystal seed in the described step 4) is 1～3%, and the intensification temperature is 80 ℃～100 ℃, and the precipitation time is 30～40 minutes.
The invention has the beneficial effects as follows: because the present invention carries out synthetic being put in the vanadium settling tank of ammonium sulfate, to be used for earlier joining in the vanadium settling tank with the sulfuric acid of ammoniacal liquor in batches, ammoniacal liquor is joined in the vanadium settling tank more in batches, and the pH that guarantees solution in whole ammonification process is less than 7, the generation so have no irritating odor in operating process helps health of operators.The present invention adopts ammoniacal liquor as precipitation agent production high-density ammonium poly-vanadate, can reduce the production cost of vanadium greatly, significantly improves economic benefit of enterprises.Used raw and auxiliary material all is a liquid, can use pipeline to be input to and contain in the vanadium solution, easily is automated control, reduces working strength of workers.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1
With concentration in the vanadium settling tank is that 27.60g/l (calculating with vanadiumcontent), temperature are that 70 ℃, pH are 9.8 the vanadium solution that contains, add concentration and be the pH to 3.17 of 96% sulfuric acid regulation solution, V sulfuric acid and V ammoniacal liquor have been calculated by above-mentioned formula, be divided into trisection, by adding the order that adds ammoniacal liquor behind the sulfuric acid earlier, being divided into for three steps joins it and contains in the vanadium solution, does not have ammonia to overflow in the ammonification process.The pH to 2.1 that adds sulfuric acid regulation solution again adds total vanadium amount and is 2% active ammonium poly-vanadate crystal seed, and elevated temperature begins precipitation, pick up counting to 96 ℃, stop heating after 40 minutes, solution is filtered, the oven dry after washing of ammonium poly-vanadate precipitation, surveying its density is 0.72g/cm
3, the deposition rate of vanadium is 98.54%.
Embodiment 2
With concentration in the vanadium settling tank is that 22.96g/l (calculating with vanadiumcontent), temperature are that 72 ℃, pH are 9.88 the vanadium solution that contains, and adds concentration and be the pH to 3.18 of 96% sulfuric acid regulation solution, has calculated V by above-mentioned formula
Sulfuric acidAnd V
Ammoniacal liquor, be divided into trisection, by adding the order that adds ammoniacal liquor behind the sulfuric acid earlier, be divided into for three steps it is joined to contain in the vanadium solution, the ammonification process does not have ammonia to overflow.The pH to 2.28 that adds sulfuric acid regulation solution again adds total vanadium amount and is 3% active ammonium poly-vanadate crystal seed, and elevated temperature begins precipitation, pick up counting to 98 ℃, stop heating after 40 minutes, solution is filtered, the oven dry after washing of ammonium poly-vanadate precipitation, surveying its density is 0.63g/cm
3, the deposition rate of vanadium is 98.85%.
Embodiment 3
With concentration in the vanadium settling tank is that 34.2g/l (calculating with vanadiumcontent), temperature are that 75 ℃, pH are 9.98 the vanadium solution that contains, add concentration and be the pH to 3.84 of 97% sulfuric acid regulation solution, V sulfuric acid and V ammoniacal liquor have been calculated by above-mentioned formula, be divided into trisection, by adding the order that adds ammoniacal liquor behind the sulfuric acid earlier, being divided into for three steps joins it and contains in the vanadium solution, and the ammonification process does not have ammonia to overflow.The pH to 2.38 that adds sulfuric acid regulation solution again adds total vanadium amount and is 2.5% active ammonium poly-vanadate crystal seed, and elevated temperature begins precipitation, pick up counting to 80 ℃, stop heating after 40 minutes, solution is filtered, the oven dry after washing of ammonium poly-vanadate precipitation, surveying its density is 0.64g/cm
3, the deposition rate of vanadium is 99.32%.
Embodiment 4
With concentration in the vanadium settling tank is that 24.99g/L (in vanadiumcontent), temperature are that 73 ℃, pH are 9.82 the vanadium solution that contains, add concentration and be the pH to 3.91 of 98% sulfuric acid regulation solution, V sulfuric acid and V ammoniacal liquor have been calculated by above-mentioned formula, be divided into the quartern, by adding the order that adds ammoniacal liquor behind the sulfuric acid earlier, being divided into for four steps joins it and contains in the vanadium solution, and the ammonification process does not have ammonia to overflow.The pH to 2.40 that adds sulfuric acid regulation solution again adds total vanadium amount and is 1% active ammonium poly-vanadate crystal seed, and elevated temperature begins precipitation, pick up counting to 90 ℃, stop heating after 40 minutes, solution is filtered, the oven dry after washing of ammonium poly-vanadate precipitation, surveying its density is 0.61g/cm
3, the deposition rate of vanadium is 99.54%.
Claims (9)
1, a kind of method for preparing the high-density ammonium poly-vanadate is characterized in that: said method comprising the steps of:
1) will contain vanadium solution, adding the sulphur acid for adjusting pH value is 2.5～5.0,
2) sulfuric acid that will add and ammoniacal liquor are divided into trisection at least, and earlier sulfuric acid was divided into at least three steps to join and contain in the vanadium solution, and then ammoniacal liquor was divided into at least three steps joins and contain in the vanadium solution,
3) the pH value 1.8～2.5 of adding sulfuric acid regulation solution,
4) add active ammonium poly-vanadate crystal seed, after the intensification precipitation, filter, after the washing, oven dry promptly.
2, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: the concentration that contains vanadium in the vanadium solution in the described step 1) is 20～40g/l.
3, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: the temperature that contains vanadium solution in the described step 1) is 70 ℃～90 ℃.
4, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: sulfuric acid concentration is 96%～98% in the described step 1).
5, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: the add-on of sulfuric acid and ammoniacal liquor is calculated by following formula described step 2):
NH wherein
3/ V=0.5～0.65.
6, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: the NH of ammoniacal liquor described step 2)
3Concentration is 18%～30%.
7, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: total vanadium amount of the active ammonium poly-vanadate crystal seed in the described step 4) is 1～3%.
8, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: the intensification temperature in the described step 4) is 80 ℃～100 ℃.
9, according to the described method for preparing the high-density ammonium poly-vanadate of claim 1, it is characterized in that: the precipitation time in the described step 4) is 30～40 minutes.
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| CNB2004100400123A CN1294084C (en) | 2004-06-17 | 2004-06-17 | Method of preparing high density ammonium polyvanadate |
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|---|---|---|---|
| CNB2004100400123A CN1294084C (en) | 2004-06-17 | 2004-06-17 | Method of preparing high density ammonium polyvanadate |
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| CN1594106A CN1594106A (en) | 2005-03-16 |
| CN1294084C true CN1294084C (en) | 2007-01-10 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100355660C (en) * | 2006-04-11 | 2007-12-19 | 华东师范大学 | Process for preparing ammonium trivanadate |
| CN102372304B (en) * | 2010-08-18 | 2013-04-17 | 河北钢铁股份有限公司承德分公司 | Physical preparation method of high density vanadium oxide powder |
| CN102502823B (en) * | 2011-10-21 | 2014-03-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for preparing high-tap density ammonium poly-vanadate |
| 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 |
| CN105236484A (en) * | 2015-10-20 | 2016-01-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of ammonium polyvanadate |
| CN106006732B (en) * | 2016-08-05 | 2017-10-24 | 攀钢集团攀枝花钢铁研究院有限公司 | The method that high concentration vanadium liquid prepares ammonium poly-vanadate |
| CN106430305B (en) * | 2016-08-31 | 2018-02-09 | 大连博融新材料股份有限公司 | A kind of production method of high density ammonium metavanadate |
| CN110029224A (en) * | 2019-05-31 | 2019-07-19 | 宜昌银钒科技有限公司 | A kind of environment friendly and pollution-free vanadic anhydride high efficiency extraction technique |
| CN113233503A (en) * | 2021-05-27 | 2021-08-10 | 河钢承德钒钛新材料有限公司 | Method for improving purity of ammonium polyvanadate |
| CN114229893B (en) * | 2021-12-10 | 2023-08-04 | 河钢承德钒钛新材料有限公司 | Preparation method of ammonium polyvanadate |
| CN115594221B (en) * | 2022-11-15 | 2024-03-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing flaky high-density ammonium polyvanadate from low ammonium content in vanadium liquid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4551315A (en) * | 1984-11-26 | 1985-11-05 | Chevron Research Company | Recovering vanadium values from ammonium bicarbonate solution |
| US4788044A (en) * | 1986-07-17 | 1988-11-29 | Ente Minerario Siciliano | Method for recovering vanadium from residues from the combustion of petroleum fractions |
| CN1056853A (en) * | 1990-05-29 | 1991-12-11 | 国营灯塔化工厂 | A kind of production method of Vanadium Pentoxide in FLAKES |
| CN1258642A (en) * | 1998-12-29 | 2000-07-05 | 攀枝花攀宏钒制品有限公司 | Continuous precipitation process of prodcing globular ammonium polyvanadate |
-
2004
- 2004-06-17 CN CNB2004100400123A patent/CN1294084C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4551315A (en) * | 1984-11-26 | 1985-11-05 | Chevron Research Company | Recovering vanadium values from ammonium bicarbonate solution |
| US4788044A (en) * | 1986-07-17 | 1988-11-29 | Ente Minerario Siciliano | Method for recovering vanadium from residues from the combustion of petroleum fractions |
| CN1056853A (en) * | 1990-05-29 | 1991-12-11 | 国营灯塔化工厂 | A kind of production method of Vanadium Pentoxide in FLAKES |
| CN1258642A (en) * | 1998-12-29 | 2000-07-05 | 攀枝花攀宏钒制品有限公司 | Continuous precipitation process of prodcing globular ammonium polyvanadate |
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