CN104745828A - Method for improving leaching rate of calcification roasting vanadium slag and improving filtering effect - Google Patents
Method for improving leaching rate of calcification roasting vanadium slag and improving filtering effect Download PDFInfo
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- CN104745828A CN104745828A CN201510174919.7A CN201510174919A CN104745828A CN 104745828 A CN104745828 A CN 104745828A CN 201510174919 A CN201510174919 A CN 201510174919A CN 104745828 A CN104745828 A CN 104745828A
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- vanadium
- slag
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a method for improving the leaching rate of calcification roasting vanadium slag and improving the filtering effect. The method comprises the following steps: (1) crushing the vanadium slag subjected to calcification roasting, and then fully mixing the vanadium slag with water to prepare ore slurry; (2) adjusting the acidity of the ore slurry by using sulfuric acid so as to perform leaching on the vanadium slag subjected to calcification roasting; (3) filtering to separate the ore slurry after leaching so as to obtain vanadium leachate and to-be-washed tailings; and (4) performing drip washing on the to-be-washed tailings by using water, and collecting the slag washing water. The method has the improvement that a small amount of a leaching additive namely polyacrylic acid, sodium citrate, polydimethylsiloxane, potassium sodium tartrate or urea is also added in the ore slurry in the step (1). Compared with the prior art, the method provided by the invention has the advantages that the vanadium leachate is increased, the vanadium leaching rate is improved, and the output-input ratio for recycling the slag washing water is relatively high.
Description
Technical field
The present invention relates to and acidleach is carried out to calcification vanadium slag sintering, to produce the method for vanadium leachate.
Background technology
Vanadium is a kind of important strategic resource, and barium oxide has multiple use, is widely used in the field such as catalysis, energy storage.One of main raw material of industrial production barium oxide is vanadium slag, and traditional technique is sodium roasting water logging vanadium extracting method.Along with the exploitation of new technology, the acid-leaching vanadium-extracted method of calcification baking is also ripe gradually, and the method is first by the oxide compound of vanadium slag and calcium or salt (CaO, CaCO
3deng) mix and carry out roasting under oxidizing atmosphere, to obtain containing acid soluble calcium vanadate (CaV
2o
6, Ca
3v
2o
8deng) calcification vanadium slag sintering; Then calcification vanadium slag sintering mixed with water and be mixed with ore pulp, then using sulfuric acid (H
2sO
4) leach for leaching agent; Filter after leaching to realize solid-liquid separation, obtain the vanadium leachate that can be used for vanadium extraction (precipitation) and the tailings that will remove; Finally carry out vanadium extraction with vanadium leachate again---be in most cases extract the widest Vanadium Pentoxide in FLAKES (V of its purposes
2o
5).Publication number is CN101161831A, " a kind of method of calcification vanadium slag sintering " by name is exactly one of these class methods.But, because the vanadium slag through calcification baking is when reacting with sulfuric acid, a large amount of unformed calcium sulfate (gypsum) will be generated in ore pulp, there is very large stickiness, this not only by part calcium vanadate to wrapping up, stop vanadium and sulfuric acid reaction, causing the leaching yield of vanadium on the low side, and also having quite a few vanadium leachate to be contained in again in the very large tailings of stickiness, this result in again the filtration difficulty for isolating vanadium leachate.So the prior art is just had in the end " washing residue 5 times ".So, not only increase time cost because needing to wash for 5 times, also increase materials cost because water total amount is comparatively large, in brief, the ratio for input and output of the prior art is relatively low.
Summary of the invention
The object of the invention is, the raising calcification vanadium slag sintering leaching yield providing a kind of ratio for input and output relatively high and the method improving filter effect.
For the technical scheme realizing described object is a kind of like this method improving calcification vanadium slag sintering leaching yield and improve filter effect.Aspect same as the prior art is that the method has the following steps:
(1) ore pulp is mixed with by fully mixing with water after the vanadium slag pulverizing of calcification baking; (2) regulate ore pulp acidity to leach the vanadium slag through calcification baking with sulfuric acid; (3) ore pulp after filtering separation leaching, obtains vanadium leachate and tailings to be washed; (4) with tailings to be washed described in water wash, and slag washing water is collected.Its improvements are:
When there being the slag washing water collected in step (4), with the water in slag washing water alternative steps (1); When the proportioning of described vanadium slag and slag washing water does not meet 0.2 ~ 2kg/L, supplement with water;
In the ore pulp described in step (1), also added additive to extraction, described additive to extraction is polyacrylic acid, Trisodium Citrate, polydimethylsiloxane, Seignette salt or urea; The consumption of additive to extraction in mass, is 0.004% ~ 1% of described vanadium slag quality;
The pH value of ore pulp acidity is regulated to be 1.5 ~ 3.5 with described sulfuric acid in step (2); Described leaching is carried out under 20 ~ 80 DEG C of conditions.
As can be seen from this programme, the present invention before with sulfuric acid to leach, with the addition of a small amount of additive to extraction in ore pulp.Added additive to extraction is a kind of hydrophobic material, and it can define one deck hydrophobic membrane at ore pulp particle surface and pore inwall, and the character of ore pulp particle surface is changed, and increases the contact angle of ore pulp particle surface and water.So, the stickiness of calcium sulfate in ore pulp can either be reduced, increase the leaching yield of vanadium; Reverse osmosis enters in the gap between ore pulp particle by capillary suction effect can to stop again vanadium leachate, and then makes the filtration procedure isolating vanadium leachate become very easy, water consumption when also just naturally decreasing drip washing tailings to be washed and drip washing number of times.Especially, apply the inventive method in first time, after step (4) obtains slag washing water, also these slag washing waters can be used for substituting in step (1) all water used, when only having it not enough, just add water supplementary.Both saved water consumption, and also greatly reduced wastewater discharge and be conducive to environmental protection.In brief, ratio for input and output of the present invention is greatly improved relative to prior art.
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment
Improve calcification vanadium slag sintering leaching yield and the method improving filter effect, the method has the following steps:
(1) ore pulp is mixed with by fully mixing with water after vanadium slag (practise and claiming: the grog) pulverizing of calcification baking; (2) regulate ore pulp acidity to leach the vanadium slag through calcification baking with sulfuric acid; (3) ore pulp after filtering separation leaching, obtains vanadium leachate and tailings to be washed; (4) with tailings to be washed described in water wash, and slag washing water is collected;
Under normal circumstances, the particle diameter of the vanadium slag through calcification baking after pulverizing, is not more than 0.12mm and is advisable.In the present invention:
When there being the slag washing water collected in step (4), with the water in slag washing water alternative steps (1); When the proportioning of described vanadium slag and slag washing water does not meet 0.2 ~ 2kg/L, supplement with water;
In the ore pulp described in step (1), also added additive to extraction, described additive to extraction is polyacrylic acid [(C
3h
4o
2)
n], Trisodium Citrate (Na
3c
6h
5o
7), polydimethylsiloxane (C
6h
18oSi2), Seignette salt (KNaC4H4O64H2O) or urea [(NH
2)
2cO]; The consumption of additive to extraction in mass, is 0.004% ~ 1% of described vanadium slag quality;
The pH value of ore pulp acidity is regulated to be 1.5 ~ 3.5 with described sulfuric acid in step (2); Described leaching is carried out under 20 ~ 80 DEG C of conditions.
Further, in the vanadium slag through calcification baking, the mass percent of content of vanadium is 1% ~ 20%, and the mass percent of calcium contents is 0.8% ~ 25%.Content of vanadium in the vanadium slag of calcification baking and calcium contents are in above-mentioned scope, the raising of V leaching rate and the improvement of filter effect, more obviously.
The present invention have passed the comparative tests checking done in laboratory.In view of except with the addition of a small amount of additive to extraction, the rest part of the inventive method is substantially identical with prior art, so be just only used as comparative example with the experiment not adding additive to extraction during contrast verification, all the other verification steps are identical with the step of above-mentioned embodiment.
During checking, all each examples are all with the vanadium slag 500g through calcification baking, and proportioning during preparation ore pulp is described identical with step (1); Regulate ore pulp acidity with sulfuric acid in step (2) after, the time leached the vanadium slag through calcification baking is 1 hour (to guarantee having comparability); The judging criterion that step (4) drip washing terminates is, when to observe with the naked eye slag washing water be colorless state, all no longer continues drip washing.
During checking, X-ray fluorescence spectra assay is utilized to leach the massfraction W of vanadium in front slag
1, and the massfraction W of vanadium in slag after washery slag
2, then weigh the mass M of slag after washery slag
2, then be calculated as follows out the leaching yield of vanadium.
The result sees the following form (note: in proof list, " to 1 " ~ " to 5 " represent each comparative example, and " example 1 " ~ " example 25 " represents each checking example; Polyacrylic acid in concrete additive to extraction, Trisodium Citrate, polydimethylsiloxane, Seignette salt and urea are in turn represented respectively by " A1 " ~ " A5 "; " content of vanadium " and " calcium contents " represents the mass percent of Vanadium in Vanadium Residue content through calcification baking and the mass percent of calcium contents respectively; " additive to extraction addition " represents additive to extraction consumption used and the mass percent through the vanadium slag of calcification baking; " solid-to-liquid ratio " represents the ratio of the vanadium slag through calcification baking in ore pulp and water or slag washing water or slag washing water+water; " slag washing water consumption " time that represents that to be observed visually slag washing water be colorless state institute's water total amount; " leach liquor volume " is gained leach liquor volume after leaching slurry filtration.)
Proof list 1:
Contrast verification table 2:
Contrast verification table 3:
Contrast verification table 4:
Contrast verification table 5:
As can be seen from contrast verification table, after employing method of the present invention, effectively increase the volume of leach liquor, prove that filter effect when isolating leach liquor obtains larger improvement, corresponding V leaching rate also obtains larger raising; Total consumption of slag washing water not only decreases, and can also recycle, and therefore, ratio for input and output is really higher than prior art.
Claims (2)
1. improve calcification vanadium slag sintering leaching yield and the method improving filter effect, the method has the following steps:
(1) ore pulp is mixed with by fully mixing with water after the vanadium slag pulverizing of calcification baking; (2) regulate ore pulp acidity to leach the vanadium slag through calcification baking with sulfuric acid; (3) ore pulp after filtering separation leaching, obtains vanadium leachate and tailings to be washed; (4) with tailings to be washed described in water wash, and slag washing water is collected; It is characterized in that:
When there being the slag washing water collected in step (4), with the water in slag washing water alternative steps (1); When the proportioning of described vanadium slag and slag washing water does not meet 0.2 ~ 2 kg/L, supplement with water;
In the ore pulp described in step (1), also added additive to extraction, described additive to extraction is polyacrylic acid, Trisodium Citrate, polydimethylsiloxane, Seignette salt or urea; The consumption of additive to extraction in mass, is 0.004% ~ 1% of described vanadium slag quality;
The pH value of ore pulp acidity is regulated to be 1.5 ~ 3.5 with described sulfuric acid in step (2); Described leaching is carried out under 20 ~ 80 DEG C of conditions.
2. improve calcification vanadium slag sintering leaching yield and the method improving filter effect according to claim 1, it is characterized in that, in the vanadium slag through calcification baking, the mass percent of content of vanadium is 1% ~ 20%, and the mass percent of calcium contents is 0.8% ~ 25%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510174919.7A CN104745828A (en) | 2015-04-14 | 2015-04-14 | Method for improving leaching rate of calcification roasting vanadium slag and improving filtering effect |
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|---|---|---|---|
| CN201510174919.7A CN104745828A (en) | 2015-04-14 | 2015-04-14 | Method for improving leaching rate of calcification roasting vanadium slag and improving filtering effect |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105886786A (en) * | 2016-05-06 | 2016-08-24 | 重庆大学 | Method for strengthening vanadium extraction from vanadium slags of converter through calcification |
| CN106048227A (en) * | 2016-06-24 | 2016-10-26 | 攀钢集团攀枝花钢钒有限公司 | Method for efficiently recycling vanadium in vanadium-containing underflow slag |
| CN106967881A (en) * | 2017-05-26 | 2017-07-21 | 江西理工大学 | A kind of method of the Extraction of rare earth from weathered superficial leaching rare-earth ore |
| CN109161695A (en) * | 2018-09-29 | 2019-01-08 | 成都先进金属材料产业技术研究院有限公司 | The method of calcification vanadium slag sintering Selectively leaching vanadium |
| CN106957961B (en) * | 2017-05-26 | 2019-01-29 | 江西理工大学 | A method of recovering rare earth and aluminium from weathered superficial leaching rare-earth ore |
| CN109517996A (en) * | 2019-01-07 | 2019-03-26 | 合肥工业大学 | A kind of technique that auxiliary agent strengthens iron in acid-hatching of young eggs extraction pyrite cinder |
| CN114350982A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by using calcified roasting clinker and recycling leaching washing liquid |
-
2015
- 2015-04-14 CN CN201510174919.7A patent/CN104745828A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105886786A (en) * | 2016-05-06 | 2016-08-24 | 重庆大学 | Method for strengthening vanadium extraction from vanadium slags of converter through calcification |
| CN106048227A (en) * | 2016-06-24 | 2016-10-26 | 攀钢集团攀枝花钢钒有限公司 | Method for efficiently recycling vanadium in vanadium-containing underflow slag |
| CN106967881A (en) * | 2017-05-26 | 2017-07-21 | 江西理工大学 | A kind of method of the Extraction of rare earth from weathered superficial leaching rare-earth ore |
| CN106967881B (en) * | 2017-05-26 | 2018-12-04 | 江西理工大学 | A method of the Extraction of rare earth from weathered superficial leaching rare-earth ore |
| CN106957961B (en) * | 2017-05-26 | 2019-01-29 | 江西理工大学 | A method of recovering rare earth and aluminium from weathered superficial leaching rare-earth ore |
| CN109161695A (en) * | 2018-09-29 | 2019-01-08 | 成都先进金属材料产业技术研究院有限公司 | The method of calcification vanadium slag sintering Selectively leaching vanadium |
| CN109161695B (en) * | 2018-09-29 | 2020-06-09 | 成都先进金属材料产业技术研究院有限公司 | Method for selectively leaching vanadium from calcified roasted vanadium slag |
| CN109517996A (en) * | 2019-01-07 | 2019-03-26 | 合肥工业大学 | A kind of technique that auxiliary agent strengthens iron in acid-hatching of young eggs extraction pyrite cinder |
| CN109517996B (en) * | 2019-01-07 | 2020-08-07 | 合肥工业大学 | Process for extracting iron in sulfuric acid cinder by aid of enhanced acid leaching method |
| CN114350982A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by using calcified roasting clinker and recycling leaching washing liquid |
| CN114350982B (en) * | 2021-11-30 | 2023-09-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium and recycling leaching washing liquid by calcified roasting clinker |
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