CN103803649A - Method for settling vanadium by using acidic vanadium solution - Google Patents
Method for settling vanadium by using acidic vanadium solution Download PDFInfo
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- CN103803649A CN103803649A CN201410069942.5A CN201410069942A CN103803649A CN 103803649 A CN103803649 A CN 103803649A CN 201410069942 A CN201410069942 A CN 201410069942A CN 103803649 A CN103803649 A CN 103803649A
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Abstract
The invention discloses a method for settling vanadium by using an acidic vanadium solution. According to the method, the vanadium is settled in a hydrothermal reaction kettle by using the acidic vanadium solution as a stock solution. The content of the vanadium in the acidic vanadium solution is 5.0-50.0g/L, and the content of the impurity phosphorus is 0.02-1.90g/L. The method comprises the following steps: (1), adjusting a pH value of the acidic vanadium solution to 0.5-2.5 in one time, then placing the acidic vanadium solution in a closed hydrothermal reaction kettle; (2), raising the temperature of the acidic vanadium solution to 100-180 DEG C for molybdenum precipitation reaction; (3), after the molybdenum precipitation reaction is ended, cooling a prepared mixture solution, and filtering to obtain a polyvanadate-containing sediment; (4), drying at a temperature of 100 DEG C after washing the sediment by using water to obtain polyvanadate; (5), calcining the polyvanadate to prepare vanadium pentoxide, wherein the calcining temperature is 500-650 DEG C. Compared with the prior art, the method has the advantages that the total production cost is saved, the vanadium settling rate can always reach above 99 percent; after an ammonia salt is added in the vanadium settling process, the vanadium settling rate is further increased.
Description
Technical field
The present invention relates to prepare with acid vanadium liquid the method for Vanadium Pentoxide in FLAKES.
Background technology
Vanadium Pentoxide in FLAKES (V
2o
5) be a kind of important industrial raw material, prepare in the method for Vanadium Pentoxide in FLAKES, having one is acidic hydrolysis precipitation method.Its concrete steps are, first prepare containing vanadium solution with the mineral containing vanadium, then regulate pH and become acid vanadium liquid, precipitate to be precipitated again afterwards thing ammonium poly-vanadate ［ (NH take acid vanadium liquid as raw material
4)
2v
6o
16, finally calcine throw out and obtain the Vanadium Pentoxide in FLAKES of fuse piece shape.Because the precipitation rate (ratio of the v element in the v element in Vanadium Pentoxide in FLAKES and acid vanadium liquid) of the method is only 80%～90%, so people improve acidic hydrolysis precipitation method by the mode that increases ammonium salt again, become acid ammonium salt precipitation method.But, in acid ammonium salt precipitation method, still must very strictly be controlled at the acidity of acid vanadium liquid in precipitation ammonium poly-vanadate process, be extremely strict controlled in the concentration of ammonium salt in acid vanadium liquid in this process, therefore, just must reach control object by adding acid for many times, the mode that adds ammonium.Obviously, time cost is in this case just larger.In addition, due in the mineral such as vanadium titano-magnetite, conventionally contain some impurity including phosphorus (P), and also inevitably exist in the acid vanadium liquid of preparing.Wherein, the existence of phosphorus is larger on the impact of precipitation, and in the time that the content of phosphorus in acid vanadium liquid is greater than 0.02g/L, precipitation rate will obviously reduce.Therefore, no matter be acidic hydrolysis precipitation method or acid ammonium salt precipitation method, by phosphorus, the content in acid vanadium liquid is reduced to the operation below 0.02g/L in advance all must to increase by one, and this has caused again the increase of production cost.
Summary of the invention
The object of this invention is to provide a kind of precipitation rate higher, and the method for the lower acid vanadium liquid of the use precipitation of production cost.
The technical scheme that realizes described goal of the invention is the method for the acid vanadium liquid of a kind of like this use precipitation, and its aspect same as the prior art is that the method is carried out precipitation take acid vanadium liquid as stoste.Its improvements are that this precipitation process is carried out in hydrothermal reaction kettle; Content of vanadium in described acid vanadium liquid is 5.00～50.00g/L, and the content of foreign matter of phosphor is 0.02～1.90g/L; Its step is as follows:
(1) once acid vanadium liquid pH value is adjusted to 0.5～2.5, is then placed in airtight hydrothermal reaction kettle;
(2) acid vanadium liquid is warming up to 100 ℃～180 ℃, to carry out precipitation reaction;
(3) precipitation reaction is finished to the mixed solution of rear gained cooling, filter containing the throw out of poly vanadic acid;
(4) after water washing and precipitating thing, at 100 ℃, be dried, obtain poly vanadic acid;
(5) poly vanadic acid is calcined, to make Vanadium Pentoxide in FLAKES; Calcining temperature is 500 ℃～650 ℃.
From scheme, can find out, present method, when with acid vanadium liquid precipitation, has adopted hydro-thermal mode (this precipitation process is carried out in hydrothermal reaction kettle), and, in the time of adjustment of acidity vanadium liquid pH value, be to adopt the mode that acid adding regulates once.So the present invention has not only saved the process of the such acid adding several times of prior art and has saved time cost; The more important thing is, when containing the high acid vanadium liquid precipitation of phosphorus, can also save that prior art must the content in acid vanadium liquid be reduced to the operation below 0.02g/L by phosphorus in advance at water hot mode, this has saved again production cost further.Checking shows, is saving under the prerequisite of total production cost, and precipitation rate of the present invention still can reach more than 99%.
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment
A method for the acid vanadium liquid of use precipitation, the method is carried out precipitation take acid vanadium liquid as stoste.In the present invention, this precipitation process is carried out in hydrothermal reaction kettle; Content of vanadium in described acid vanadium liquid is 5.00～50.00g/L, and the content of foreign matter of phosphor is 0.02～1.90g/L; Its step is as follows:
(1) once acid vanadium liquid pH value is adjusted to 0.5～2.5(and it will be apparent to those skilled in that, when the pH value of adjustment of acidity vanadium liquid, conventionally all select sulfuric acid---H
2sO
4), be then placed in airtight hydrothermal reaction kettle;
(2) acid vanadium liquid is warming up to 100 ℃～180 ℃, to carry out precipitation reaction (the how many and temperature of reaction of the content of vanadium of reaction times in obviously should acid vanadium liquid is grasped, conventionally between 1.0～6.0 hours);
(3) precipitation reaction is finished to the mixed solution of rear gained cooling, filter containing the throw out of poly vanadic acid;
(4) after water washing and precipitating thing, at 100 ℃, be dried, obtain poly vanadic acid;
(5) poly vanadic acid is calcined, to make Vanadium Pentoxide in FLAKES; Calcining temperature is 500 ℃～650 ℃ (calcination time is generally 2.0～3.0 hours).
Disclose so far, those skilled in the art, completely can be how many according to the content of vanadium in concrete acid vanadium liquid in conjunction with the understanding to beneficial effect of the present invention, and how much content of foreign matter of phosphor has specifically been implemented.
For further obtaining better effect, on such scheme basis, in step (1) adjustment of acidity vanadium liquid pH value, also add and have ammonium salt, the add-on of ammonium salt is: ammonium salt quality: quality=1.0～3.0 of vanadium in acid vanadium liquid; Ammonium salt is ammonium sulfate ［ (NH
4)
2sO
4, ammonium chloride (NH
4or ammonium nitrate (NH Cl)
4nO
3).
The present invention has passed through experimental verification.
Before checking, first by the quality (content of vanadium) of ferrous ammonium sulfate titration checking contained vanadium in acid vanadium liquid, after Vanadium Pentoxide in FLAKES, weigh obtaining, according to molecular formula V
2o
5calculate the quality of the vanadium that settles out, finally calculate precipitation rate.The result is shown in proof list.
Note: in table, " phosphorus content " refers to checking phosphorous quality in acid vanadium liquid, " pH value " is with the disposable acidity value adjusting of sulfuric acid in step (1), " adding ammonium coefficient " is ammonium salt quality: the quality of vanadium in acid vanadium liquid, " temperature of reaction " and " reaction times " is the temperature and time of step (2).Be step of the prior art in view of step (5) is real, therefore its calcining temperature and time are unlisted in table.
Proof list
From proof list, can find out, even if the phosphorus content in acid vanadium liquid substantially exceeds in the situation of 0.02g/L, precipitation rate of the present invention also more than 99%, add the mode of ammonium salt in conjunction with prior art after, some raising again of its precipitation rate; Add that the present invention has advantages of that with respect to prior art total production cost is low, illustrate that with regard to being enough to the present invention has improved with respect to the comprehensive benefit of prior art.
Special instruction, while being greater than 0.02g/L, adopts the just obviously reduction of precipitation rate of prior art because of the content of phosphorus in acid vanadium liquid, so, in above-mentioned checking example, do not record its phosphorus content and equal the situation of 0.02g/L.Those skilled in the art is certainly clear, in the time that the content of phosphorus in acid vanadium liquid equals 0.02g/L, is adapted to equally the present invention.
Claims (2)
1. by a method for acid vanadium liquid precipitation, the method is carried out precipitation take acid vanadium liquid as stoste, it is characterized in that: this precipitation process is carried out in hydrothermal reaction kettle; Content of vanadium in described acid vanadium liquid is 5.00～50.00g/L, and the content of foreign matter of phosphor is 0.02～1.90g/L; Its step is as follows:
(1) once acid vanadium liquid pH value is adjusted to 0.5～2.5, is then placed in airtight hydrothermal reaction kettle;
(2) described acid vanadium liquid is warming up to 100 ℃～180 ℃, to carry out precipitation reaction;
(3) precipitation reaction is finished to the mixed solution of rear gained cooling, filter containing the throw out of poly vanadic acid;
(4) after water washing and precipitating thing, at 100 ℃, be dried, obtain poly vanadic acid;
(5) poly vanadic acid is calcined, to make Vanadium Pentoxide in FLAKES; Calcining temperature is 500 ℃～650 ℃.
2. the method for using according to claim 1 the precipitation of acid vanadium liquid, is characterized in that, in step (1) adjustment of acidity vanadium liquid pH value, also adds and has ammonium salt, and the add-on of ammonium salt is: ammonium salt quality: quality=1.0～3.0 of vanadium in acid vanadium liquid; Described ammonium salt is ammonium sulfate, ammonium chloride or ammonium nitrate.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373226A (en) * | 2018-02-13 | 2018-08-07 | 洛阳理工学院 | A kind of hydro-thermal of low-concentration vanadium-containing waste water-absorption combination treatment method |
| CN109081465A (en) * | 2018-07-13 | 2018-12-25 | 绍兴齐英膜科技有限公司 | The recovery method of vanadium catalyst in pigment wastewater |
| CN109516499A (en) * | 2018-11-30 | 2019-03-26 | 攀钢集团研究院有限公司 | The method that high phosphorus solution containing vanadium produces vanadium oxide |
| CN115611310A (en) * | 2022-10-08 | 2023-01-17 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide by using vanadium-containing solution |
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| 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 |
| CN102897834A (en) * | 2011-07-29 | 2013-01-30 | 攀钢集团钢铁钒钛股份有限公司 | Vanadium-precipitating method and preparation method for vanadium pentoxide |
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| CN102897834A (en) * | 2011-07-29 | 2013-01-30 | 攀钢集团钢铁钒钛股份有限公司 | Vanadium-precipitating method and preparation method for vanadium pentoxide |
| 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373226A (en) * | 2018-02-13 | 2018-08-07 | 洛阳理工学院 | A kind of hydro-thermal of low-concentration vanadium-containing waste water-absorption combination treatment method |
| CN109081465A (en) * | 2018-07-13 | 2018-12-25 | 绍兴齐英膜科技有限公司 | The recovery method of vanadium catalyst in pigment wastewater |
| CN109516499A (en) * | 2018-11-30 | 2019-03-26 | 攀钢集团研究院有限公司 | The method that high phosphorus solution containing vanadium produces vanadium oxide |
| CN109516499B (en) * | 2018-11-30 | 2021-04-27 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide from high-phosphorus vanadium-containing liquid |
| CN115611310A (en) * | 2022-10-08 | 2023-01-17 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide by using vanadium-containing solution |
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Application publication date: 20140521 |