CN107416900A - A kind of method for efficiently preparing high-purity sodium metavanadate - Google Patents
A kind of method for efficiently preparing high-purity sodium metavanadate Download PDFInfo
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- CN107416900A CN107416900A CN201710771512.1A CN201710771512A CN107416900A CN 107416900 A CN107416900 A CN 107416900A CN 201710771512 A CN201710771512 A CN 201710771512A CN 107416900 A CN107416900 A CN 107416900A
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- sodium
- sodium metavanadate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to field of metallurgy, and in particular to a kind of preparation method of sodium metavanadate.The technical problem to be solved in the present invention is to provide a kind of method for efficiently preparing high-purity sodium metavanadate, this method comprises the following steps：A, sulfuric acid and ammonium sulfate are added into vanadium extraction leachate；B, pH value of solution is adjusted to 4~6, filtering, obtains ammonium vanadate sodium solid；C, ammonium vanadate sodium solid is added in sodium hydroxide solution, deamination, and regulation solution ph obtains sodium metavanadate solution to 8~8.5；D, sodium metavanadate solution is subjected to spraying flash distillation, obtains sodium metavanadate solid.The inventive method can prepare high-purity sodium metavanadate, sodium metavanadate crystalline rate and yield significantly improve, and sodium metavanadate purity ＞ 99.5%, crystallize direct yield ＞ 99%, crystalline rate improves 35% compared with evaporating, concentrating and crystallizing, and product quality is stable.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of method for efficiently preparing high-purity sodium metavanadate.
Background technology
The fine chemical product of vanadium mainly has sodium metavanadate/potassium/ammonium, sulfuric acid/vanadyl oxalate, mainly for the manufacture of catalyst
(such as sulfuric acid industry, power-plant flue gas denitration).Vanadium has special catalytic activity, and other elements are difficult to replace, and the whole world is about
4%~5% vanadium product application is in this.
Traditional sodium metavanadate preparation method is with sodium hydroxide solution dissolving powdery five oxidation two under conditions of heating
Sodium vanadate solution is obtained after vanadium, fully reaction, sodium metavanadate is then prepared by evaporative crystallization.This method is simple to operate, no
Pollution waste gas (ammonia) is produced, is to use relatively broad method at present, but this method will to the quality of powdery vanadic anhydride
Ask higher, while industrial powdered vanadic anhydride price is costly, production cost is high.Another method is to remove vanadium extraction leachate
Evaporative crystallization after miscellaneous, so as to obtain sodium metavanadate solid, this method technique is simple, easy to operate, but vanadium extraction ammonium acetate
Complexity, go the removal of impurity incomplete by crystallization, cause product purity ＜ 97%, be not used widely.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of cheap efficient preparation high-purity sodium metavanadate of cost
Method.
Technical scheme there is provided a kind of preparation method of sodium metavanadate used by the present invention solves above-mentioned technical problem,
This method comprises the following steps：
A, sulfuric acid and ammonium sulfate are added into vanadium extraction leachate；
B, pH value of solution is adjusted to 4~6, filtering, obtains ammonium vanadate sodium solid；
C, ammonium vanadate sodium solid is added in sodium hydroxide solution, deamination, and regulation solution ph obtains metavanadic acid to 8~8.5
Sodium solution；
D, sodium metavanadate solution is subjected to spraying flash distillation, obtains sodium metavanadate solid.
Wherein, in the above method, in step a, the vanadium concentration of the vanadium extraction leachate is 20~50g/L, silicon concentration 1.0
~6.0g/L, chromium concn are 2.0~8.0g/L.
Wherein, in the above method, in step a, the addition of the sulfuric acid is to adjust pH value of solution to 6~7.
Wherein, in the above method, in step a, the ammonium sulfate is 0.8~1.5 with vanadium mass ratio in solution：1.
Wherein, in the above method, in step b, using sulfuric acid regulation solution pH.
Wherein, in the above method, in step a and b, the concentration of the sulfuric acid is 2~5mol/L.
Wherein, in the above method, in step c, the concentration of the sodium hydroxide solution is 60~80g/L.
Wherein, in the above method, in step c, the deamination stirs, deaerated to be heated to seething with excitement.
Wherein, in the above method, in step c, after deamination, the acid steady liquor regulation pH value of benefit to 8~8.5, the acidity
Steady liquor is high-purity vanadium pentoxide.
Wherein, in the above method, in step d, it is described spraying flash distillation temperature be 80~120 DEG C, inlet amount be 40~
60mL/min。
The beneficial effects of the invention are as follows：
The present invention control ammonium vanadate sodium crystalline solid form precipitation, avoids impurity from wrapping up, avoids and carry by adjusting solution acidity
Influence of the impurity such as silicon, chromium to ammonium vanadate sodium in vanadium leachate, it is thus possible to obtain pure height sodium metavanadate solution, enter without
Filtering or condensing crystallizing are used, but uses spraying flash distillation, sodium metavanadate crystalline rate and yield significantly improve, purity ＞
99.5%, direct yield ＞ 99% is crystallized, crystalline rate improves 35% compared with evaporating, concentrating and crystallizing, while eliminates calcining V2O5's
Step；The inventive method reaction condition is gentle, and technique is simple, and cost reduces, and gained sodium metavanadate crystal size is uniform, product matter
Amount is stable.
Brief description of the drawings
The process flow diagram of Fig. 1 the inventive method
Embodiment
A kind of preparation method of sodium metavanadate, this method comprise the following steps：
A, sulfuric acid and ammonium sulfate are added into vanadium extraction leachate；
B, pH value of solution is adjusted to 4~6, filtering, obtains ammonium vanadate sodium solid；
C, ammonium vanadate sodium solid is added in sodium hydroxide solution, deamination, and regulation solution ph obtains metavanadic acid to 8~8.5
Sodium solution；
D, sodium metavanadate solution is subjected to spraying flash distillation, obtains sodium metavanadate solid.
The present invention use vanadium extraction leachate, and for vanadium titano-magnetite leaching vanadium solution, its vanadium concentration is 20~50g/L, silicon concentration
For 1.0~6.0g/L, chromium concn is 2.0~8.0g/L；Si significantly affects sodium metavanadate clarity of solution, is unfavorable for sodium metavanadate
Solution disperses；Sexavalence Cr is poisonous and harmful element, not only significantly affects activity of the sodium metavanadate as catalyst, or environmental protection weight
Point monitoring, content is more low better.
The inventive method first adds sulfuric acid regulation solution pH to 6~7 in step a, then added by adjusting solution acidity
Ammonium sulfate, sulfuric acid regulation solution pH to 4~6 is added in step b, control ammonium vanadate sodium crystalline solid form precipitation, avoids impurity bag
Wrap up in, avoid influence of the impurity such as silicon in solution, chromium to ammonium vanadate sodium, to obtain high-purity sodium metavanadate molten so as to subsequent step c
Liquid.The concentration of the sulfuric acid is 2~5mol/L, and the ammonium sulfate is 0.8~1.5 with vanadium mass ratio in solution：1.
Key reaction equation：
5Na4V2O7+2(NH4)2SO4+7H2SO4=Na2(NH4)4V10O28↓+9Na2SO4+7H2O (normal temperature)
In step c, the concentration of the sodium hydroxide solution is 60~80g/L, and now sodium metavanadate is best in quality, sprays simultaneously
Mist flash distillation energy consumption is low, more economical；Concentration of sodium hydroxide solution is too high, and solution is too sticky, easy blocking sprayer；It is too low, then it can increase
It is spray-dried energy consumption, it is also possible to cause material moisture increase after spray drying；The dosage of sodium hydroxide solution is mended according to follow-up
After acid steady liquor, regulation solution ph determines to 8~8.5, can typically use sodium hydroxide solution and vanadium extraction extracted liquid
Product is than being 0.8~2：3.
In step c, the deamination stirs, deaerated, ammonia is absorbed using the concentrated sulfuric acid, is obtained to be heated to seething with excitement
Ammonium sulfate can be recycled；Due to vanadic acid root, polymeric species are relevant under the conditions of different acidity, after deamination, mend acid steady liquor and adjust
PH value is saved to 8~8.5, now vanadic acid root is metavanadic acid root, and spray drying effect is best；The acid steady liquor is high-purity five
V 2 O.
Key reaction equation：
Na2(NH4)4V10O28+ 8NaOH=10NaVO3+4NH3↑+6H2O
Because sodium metavanadate solution purity is high, flashed using spraying, crystalline rate and yield can be significantly improved, save life
Produce the time, the temperature of the spraying flash distillation is 80~120 DEG C, and inlet amount is 40~60mL/min.
Optimization, the inventive method can be implemented in such a way：
A, it is 20~50g/L to vanadium concentration, silicon concentration is 1.0~6.0g/L, and the vanadium extraction that chromium concn is 2.0~8.0g/L is soaked
Go out and sulfuric acid and ammonium sulfate are added in liquid, the wherein concentration of sulfuric acid is 2~5mol/L, and sulphuric acid is to adjust pH value of solution to 6~7
It is defined, ammonium sulfate is 0.8~1.5 with vanadium mass ratio in solution：1；
B, 2~5mol/L sulfuric acid regulation solution pH value is added to 4~6, filtering, obtains ammonium vanadate sodium solid；
C, ammonium vanadate sodium solid is added in 60~80g/L sodium hydroxide solutions, is heated to seething with excitement, stirs, deaerate, mend acid
Property steady liquor adjust pH value to 8~8.5, obtain high-purity sodium metavanadate solution, the acid steady liquor is that high-purity five aoxidizes
Two vanadium；
D, sodium metavanadate solution is subjected to spraying flash distillation, drying temperature is 80~120 DEG C, and inlet amount is 40~60mL/
Min, obtain sodium metavanadate solid.
The present invention is described in further detail below by embodiment, but therefore not limited the scope of the present invention
Among described scope of embodiments.
1+4 dilute sulfuric acids described in embodiment is the concentrated sulfuric acid for 98% mass concentration for taking 1 parts by volume, the water with 4 parts by volume
Mixing, is formulated, its concentration is about 3.7mol/L.
Embodiment 1
Vanadium extraction leachate 3L, [V] 35.2g/L, [Si] 1.8g/L, [Cr] 2.5g/L are taken, adds volume ratio 1+4 dilute sulfuric acids,
PH value 6.43 is adjusted, 100g ammonium sulfate is added, adds 1+4 dilute sulfuric acids to pH to 5.41, be filtrated to get crocus ammonium vanadate sodium.Match somebody with somebody
1L sodium hydroxide solutions are put, naoh concentration 65g/L, after adding 250g ammonium vanadate sodium, is heated to seething with excitement, stirs, deaerates, are mended
Acid steady liquor adjusts pH value to 8.41, obtains 1.1L sodium metavanadate solution.Solution is entered using NAI-GZJ small-sized spray driers
Row spraying flash distillation, 105 DEG C, inlet amount 50mL/min of drying temperature, obtains 252.1g purity and is more than 99.6% faint yellow metavanadic acid
Sodium powder end, yield 99.4%, its Cr content 0.007%, Si contents 0.011%, Fe contents 0.004%, As, P content ＜
0.001%；Sodium metavanadate crystal size is uniform, and particle diameter is in -60~+120 mesh.
Embodiment 2
Vanadium extraction leachate 3L, [V] 23.2g/L, [Si] 1.1g/L, [Cr] 2.1g/L are taken, adds volume ratio 1+4 dilute sulfuric acids,
PH value 6.73 is adjusted, 100g ammonium sulfate is added, adds 1+4 dilute sulfuric acids to pH to 5.01, be filtrated to get crocus ammonium vanadate sodium.Match somebody with somebody
1L sodium hydroxide solutions are put, naoh concentration 75g/L, after adding 250g ammonium vanadate sodium, are heated to seething with excitement, are stirred, are deaerated, are mended
Acid steady liquor adjusts pH value to 8.32, obtains 1.2L sodium metavanadate solution.Solution is sprayed using NAI-GZJ small-sized spray driers
Mist flashes, and 105 DEG C, inlet amount 50mL/min of drying temperature, obtains 165.8g purity and is more than 99.5% faint yellow metavanadic acid sodium powder
End, yield 99.1%, its Cr content 0.006%, Si contents 0.014%, Fe contents 0.005%, As, P content ＜ 0.001%；
Sodium metavanadate crystal size is uniform, and particle diameter is in -60~+120 mesh.
Embodiment 3
Vanadium extraction leachate 3L, [V] 48.2g/L, [Si] 4.1g/L, [Cr] 5.6g/L are taken, adds volume ratio 1+4 dilute sulfuric acids,
PH value 6.83 is adjusted, 150g ammonium sulfate is added, adds 1+4 dilute sulfuric acids to pH to 4.5, be filtrated to get crocus ammonium vanadate sodium.Match somebody with somebody
1L sodium hydroxide solutions are put, naoh concentration 80g/L, after adding 300g ammonium vanadate sodium, are heated to seething with excitement, are stirred, are deaerated, are mended
Acid steady liquor adjusts pH value to 8.18, obtains 1.2L sodium metavanadate solution.Solution is sprayed using NAI-GZJ small-sized spray driers
Mist flashes, and 105 DEG C, inlet amount 50mL/min of drying temperature, obtains 345.6g purity and is more than 99.6% faint yellow metavanadic acid sodium powder
End, yield 99.5%, its Cr content 0.009%, Si contents 0.012%, Fe contents 0.005%, As, P content ＜ 0.001%；
Sodium metavanadate crystal size is uniform, and particle diameter is in -60~+120 mesh.
From embodiment 1~3, the inventive method can efficiently prepare sodium metavanadate production from the high vanadium solution of high-silicon high chromium
Product, by adjusting solution acidity, control ammonium vanadate sodium crystalline solid form precipitation, avoid impurity from wrapping up, obtain high-purity metavanadic acid
Sodium solution, therefore spraying flash distillation can be used, sodium metavanadate crystalline rate and yield significantly improve, and crystallize direct yield ＞
99%, crystalline rate improves 35% compared with evaporating, concentrating and crystallizing, while eliminates calcining V2O5The step of, prepare gained sodium metavanadate
Purity ＞ 99.5%；The inventive method reaction condition is gentle, and technique is simple, and cost is cheap, and sodium metavanadate crystal size is uniform, production
Quality is stable.
Claims (10)
1. the preparation method of sodium metavanadate, it is characterised in that：Comprise the following steps：
A, sulfuric acid and ammonium sulfate are added into vanadium extraction leachate；
B, pH value of solution is adjusted to 4~6, filtering, obtains ammonium vanadate sodium solid；
C, ammonium vanadate sodium solid is added in sodium hydroxide solution, deamination, and it is molten to obtain sodium metavanadate to 8~8.5 for regulation solution ph
Liquid；
D, sodium metavanadate solution is subjected to spraying flash distillation, obtains sodium metavanadate solid.
2. the preparation method of sodium metavanadate according to claim 1, it is characterised in that：In step a, the vanadium extraction leachate
Vanadium concentration be 20~50g/L, silicon concentration is 1.0~6.0g/L, and chromium concn is 2.0~8.0g/L.
3. the preparation method of sodium metavanadate according to claim 1 or 2, it is characterised in that：In step a, the sulfuric acid
Addition is to adjust pH value of solution to 6~7.
4. the preparation method of sodium metavanadate according to claim 1, it is characterised in that：In step a, the ammonium sulfate with it is molten
Vanadium mass ratio is 0.8~1.5 in liquid：1.
5. the preparation method of sodium metavanadate according to claim 1, it is characterised in that：In step b, adjusted using sulfuric acid molten
Liquid pH.
6. the preparation method of the sodium metavanadate according to any one of Claims 1 to 5, it is characterised in that：In step a and b, institute
The concentration for stating sulfuric acid is 2~5mol/L.
7. the preparation method of sodium metavanadate according to claim 1, it is characterised in that：In step c, the sodium hydroxide is molten
The concentration of liquid is 60~80g/L.
8. the preparation method of sodium metavanadate according to claim 1, it is characterised in that：In step c, the deamination is heating
To boiling, stirring, degassing.
9. the preparation method of sodium metavanadate according to claim 1, it is characterised in that：In step c, after deamination, mend acid
Steady liquor adjusts solution ph to 8~8.5；The acid steady liquor is high-purity vanadium pentoxide..
10. the preparation method of the sodium metavanadate according to any one of claim 1~9, it is characterised in that：It is described in step d
The temperature of spraying flash distillation is 80~120 DEG C, and inlet amount is 40~60mL/min.
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Cited By (3)
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| CN110436520A (en) * | 2019-09-11 | 2019-11-12 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing vanadium product using sodium vanadate cleaning |
| CN114164348A (en) * | 2021-09-16 | 2022-03-11 | 王仕斌 | Method for extracting vanadium in sulfuric acid leaching solution reduced by waste vanadium-poor catalyst |
| CN114275813A (en) * | 2021-12-30 | 2022-04-05 | 中国科学院过程工程研究所 | Method for flash evaporation, cooling and crystallization of sodium vanadate in alkali liquor system |
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Effective date of registration: 20180130 Address after: 617000 Panzhihua City, Sichuan Province, panping Pangang Group, the East District of Sichuan Province, vanadium and titanium group Applicant after: PANGANG GROUP STEEL VANADIUM & TITANIUM CO., LTD. Address before: 617067 Panzhihua East District of Sichuan Province, Wapu green Panzhihua Iron and Steel Group vanadium Co., Ltd. Applicant before: Pangang Group Vanadium Industry Co Ltd |
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Application publication date: 20171201 |