CN103667749A - Method for enriching scandium in anatase raw ore - Google Patents
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- CN103667749A CN103667749A CN201310740585.6A CN201310740585A CN103667749A CN 103667749 A CN103667749 A CN 103667749A CN 201310740585 A CN201310740585 A CN 201310740585A CN 103667749 A CN103667749 A CN 103667749A
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Abstract
The invention discloses a method for enriching scandium in anatase raw ore. The method comprises the following steps: 1) mixing the anatase raw ore with inorganic acid to obtain a scandium leachate and tailings; 2) mixing an extraction agent with an organic solvent and an additive, so as to obtain an organic phase; 3) extracting the scandium leachate by use of the organic phase, so as to obtain a first extract liquor; 4) washing the first extract liquor by use of a washing liquid, and then back-extracting scandium element in the first extract liquid by use of a back-extracting solution, so as to obtain a coarse scandium solution. The method disclosed by the invention can be used for improving the grade of the scandium in the raw ore by more than 150 times and ensuring that the total scandium yield is greater than 80%; back-extracting of scandium is easy, and loss of the organic phase is less; the chemical raw material consumption is less, and the method is clean and environment-friendly.
Description
Technical field
The present invention relates to the enriching method of anatase octahedrite raw ore scandium, in particular to take anatase octahedrite raw ore as raw material, first with chemical method by scandium Elements Leaching, then with solvent extration, extract the technique of scandium.
Background technology
Scandium, as one of strategic element, can be applied to high-tech area.The independent mineral reserve of scandium almost do not have, and main association is in rare-earth mineral, bauxite, iron ore, navajoite, titanium ore, tungsten ore, uranium ore etc.China reclaims scandium from contain the mineral such as scandium rare-earth mineral, titanium ore (titanium white waste acid), tungsten slag.Also there is in recent years the report that reclaims scandium from bauxite (red mud).
Li Jiucheng discloses rare-earth mineral (comprising association rare-earth mineral, rich scandium subsiliceous rock saprolite, rich scandium bauxite and red mud, mixed rare-earth oxide muriate) for raw material, select hydrochloric acid, sulfuric acid, ammonium chloride, ammonium sulfate, sodium-chlor leaching to carry scandium and rare earth mother solution, select the method (CN85106255) of the extraction process scandium-enricheds such as naphthenic acid HA, P204, P507, P350, TBP.Hunan rare earth technology company and east scandium industry disclose respectively the method (CN201010230723.2, CN201210208769.3) that P204-TBP and P507-TBP reclaim scandium titanium from titanium dioxide wastewater.Now part scandium being reclaimed to Patents enumerates in table 1:
Anatase octahedrite raw ore, weathering is comparatively complete, outward appearance is khaki color, light brown, grey, loose soil is block, containing ferric oxide approximately 20%, titanium oxide approximately 5%, particularly Scium trioxide reach 65ppm and more than, far above the Abundances (about 25ppm) of scandium in soil.The occurrence status research of scandium element shows, 86% scandium is that ionic species is adsorbed or is wrapped in the mineral such as kaolinite, limonite, has very high extraction and is worth, but there is not yet examples of industrial application.Therefore need to seek scandium-enriched in a kind of applicable anatase octahedrite raw ore, and remove the method for the impurity such as iron, aluminium, titanium.
Summary of the invention
The object of the invention is to provide the enriching method of scandium element in a kind of anatase octahedrite raw ore, take anatase octahedrite raw ore as raw material, first with chemical method by scandium Elements Leaching, then extract scandium with solvent extration.During chemical method leaching scandium, because most of scandium is ionic species, be easy to leaching; And the concentration of scandium is high in leaching liquid, reduce industrial chemicals consumption; Leaching liquid impurity is few, and extraction phenomenon is good.Specifically comprise the following steps:
1) anatase octahedrite raw ore is mixed with mineral acid, obtain scandium leach liquor and tailings;
2) extraction agent is mixed with organic solvent and additive, obtain organic phase;
3) use described organic phase to extract scandium leach liquor, obtain the first extraction liquid;
4) with washings, wash after the first extraction liquid, the scandium element of stripping in described the first extraction liquid with anti-stripping agent, obtains thick scandium solution.
Preferably, in anatase octahedrite raw ore, the grade of Scium trioxide is 40 ~ 400ppm.
Preferably, during roasted ore leaching scandium, mineral acid is selected from one or more in hydrochloric acid, nitric acid and sulfuric acid, and volumetric concentration is 5 ~ 30%.Leach liquor composition is Sc
2o
35 ~ 150ppm, TiO
20.05 ~ 5 grams per liter, Fe
2o
35 ~ 50 grams per liters, free H
+0.2 ~ 8.0 mol/L.
Preferably, described extraction agent is selected from one or more in higly branched chain hexadecyl primary amine (code name N116), heptadecyl-9-amine (code name N179), 19 ~ pentacosyl-(10 ~ 13)-amine (code name N1923), Primene JM-T; Described organic solvent is selected from one or more in sulfonated kerosene, dimethylbenzene, hexanaphthene; Described additive is selected from isooctyl alcohol or TBP; In organic phase, the volume ratio of extraction agent additive and organic solvent is 1 ~ 20:1 ~ 20:60 ~ 98.
Preferably, described washings is hydrochloric acid, nitric acid or sulfuric acid, and volumetric concentration is 0.1 ~ 4 mol/L; Described strip liquor is hydrochloric acid or nitric acid, and volumetric concentration is 0.2 ~ 4 mol/L.
Preferably, described organic phase, stock liquid, washings and anti-stripping agent throughput ratio are 0.5 ~ 1.5:2 ~ 10:0.25 ~ 2:0.25 ~ 2; Extraction progression is 1 ~ 6 grade, and washing progression is 1 ~ 6 grade; Reextraction progression is 1 ~ 6 grade.
According to of the present invention from anatase octahedrite raw ore the method for scandium-enriched, Sc in described anatase octahedrite raw ore
2o
3grade be 40 ~ 400ppm, separately containing TiO
2approximately 5%, Fe
2o
3approximately 20%, Al
2o
3approximately 23%, other component group will be silicate.Raw ore and mineral acid are mixed to get leach liquor, and standing rear supernatant liquid is as the stock liquid of extracting operation.Described mineral acid is preferably nitric acid, hydrochloric acid or sulfuric acid.In a preferred implementation, leaching rate is greater than 85%, leaches near the radioactivity of storage tank lower than 0.25 μ Sv/h, without radioactivity protection.
According to of the present invention from anatase octahedrite raw ore the method for scandium-enriched, described extraction agent is selected from one or more in N116, N179, N1923, Primene JM-T.Described organic solvent is selected from one or more in sulfonated kerosene, dimethylbenzene, hexanaphthene, more preferably sulfonated kerosene; Described additive is selected from isooctyl alcohol or TBP; In organic phase, the volume ratio of extraction agent, additive and organic solvent is 1 ~ 20:1 ~ 20:60 ~ 98, more preferably 3 ~ 8:3 ~ 8:84 ~ 94.
According to of the present invention from anatase octahedrite raw ore the method for scandium-enriched, described washings is for removing the impurity such as iron that the first extraction liquid carries secretly, titanium, it is not particularly limited, but is preferably hydrochloric acid, nitric acid or sulfuric acid, volumetric concentration is 0.1 ~ 4 mol/L.Described strip liquor, for the back extraction of the first extraction liquid scandium, makes organic phase regeneration be convenient to recycle simultaneously, is preferably hydrochloric acid or nitric acid, and concentration is 0.2 ~ 4 mol/L.
According to of the present invention from anatase octahedrite raw ore the method for scandium-enriched, for the extraction equipment of implementing fractional-distillation extraction, be not specifically limited, as long as it can realize extraction object of the present invention.Described extraction equipment can be selected equipment well known in the art, as separating funnel, mixed settler extractor, centrifugal extractor etc.In a preferred implementation, use mixed settler extractor to carry out fractionation extraction.
Fig. 1 is shown in technical process of the present invention.
As shown in Figure 1, wherein n, m, j are fractionation extraction progression sequence number, n=1 ~ 6; M=n+ (1 ~ 6); J=m+n+ (1 ~ 4).Organic phase adds from the 1st grade, and stock liquid is added by n level, and after organic extractant phase, raffinate is discharged from the 1st grade of below, washings adds from m level, and anti-stripping agent adds from j level, and the first extraction liquid after washing is stripped, obtain thick scandium, from m+1 level, discharge.Organic phase after reextraction is discharged from j level, recycle.
In this anatase octahedrite raw ore, the occurrence status of scandium element is significantly different containing scandium ore (such as ilmenite, artificial rutile) from other type, and easily, in leach liquor, the content of impurity titanium is little, is more conducive to extracting operation in leaching.In leach liquor, radioactive activity is low, to workman's operational safety.The extracting scandium different by the technique of sodium hydroxide precipitation back extraction scandium from titanium white waste acid from traditional P204 or P507, in the extraction procedure described in this patent, amine extractant extraction ability is good, and the solubleness of organic phase is little; The reextraction of scandium is easy, and organic phase loss is little, has reduced cost and has improved production efficiency.The results show, is used the inventive method can make the grade of scandium in raw ore bring up to more than 150 times, and scandium leaching rate is greater than 85%, and total recovery is greater than 80%.
Accompanying drawing explanation
The technical process of Fig. 1 scandium-enriched from anatase octahedrite raw ore.
Embodiment
In order further to understand the present invention, below the preferred embodiments of the invention are described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention rather than limiting to the claimed invention.Wherein, conventional chemical reagent is analytical pure.
Embodiment 1
Preparation raw material liquid: the anatase octahedrite raw ore of getting scandium grade and be 65ppm reacts to obtain leach liquor with dilute sulphuric acid, as the raw materials used liquid of extraction.By analysis, the composition of stock liquid is: Sc
2o
316.2ppm, TiO
20.66 grams per liter, Fe
2o
3(trivalent) 21 grams per liters, Al
2o
314 grams per liters, free H
+3.7 mol/L.
Preparation organic phase: the N1923 extraction agent of getting technical grade is dissolved in sulfonated kerosene, and adds isooctyl alcohol, and now organic phase volume consists of 5 % N1923-5% isooctyl alcohol-90% sulfonated kerosenes.
Fractionation extraction: whole extraction process adopts separating funnel simulation fractionation extraction, comprises 2 grades of extractions, 2 grades of washings and 2 grades of back extractions.Organic phase adds from the 1st grade; Stock liquid adds from the 2nd grade; Washings adopts 0.5 mol/L sulfuric acid, from the 4th grade, adds; Anti-stripping agent adopts 1.0 mol/L hydrochloric acid, from the 6th grade, adds.The throughput ratio of organic phase, stock liquid, washings, anti-stripping agent is 1:4:0.5:0.3.Mixing time is 8 minutes.Enrichment through this flow process, obtains thick scandium solution, and extraction yield reaches 97%, and in raw ore, the grade of scandium has improved 160 times.Scandium leaching rate is greater than 85%, and total recovery is greater than 82%.Thick scandium solution obtains thick scandium cake through alkali precipitation, and through chemical analysis, scandium accounts for 2.5%, and iron accounts for 95%.Organic phase recycles, and extraction ability is stable, carries secretly with solution loss little.
Embodiment 2
Preparation raw material liquid: get scandium grade and be the anatase octahedrite raw ore leach liquor of 105ppm as stock liquid, its composition is: Sc
2o
343ppm, TiO
20.14 grams per liter, ferrous sulfate is (with Fe
2o
3meter) 33 grams per liters, Al
2o
318 grams per liters, free H
+3.1 mol/L.
Preparation organic phase: the N1923 extraction agent of getting technical grade is dissolved in sulfonated kerosene, and adds additive TBP, and now organic phase volume consists of 5 % N1923-5%TBP-90% sulfonated kerosenes.
Fractionation extraction: whole extraction process adopts mixed settler extractor to carry out fractionation extraction, extraction progression is adjusted into 4 grades of extractions, 3 grades of washings and 3 grades of back extractions.Washings is 0.1 mol/L hydrochloric acid, and anti-stripping agent adopts 80 grams per liter aqueous sodium hydroxide solutions.The throughput ratio of organic phase, stock liquid, washings, anti-stripping agent is 1:5:0.5:0.25.Mixing time is 8 minutes.Through the enrichment of this flow process, total recovery is greater than 85%.
In the present embodiment, the composition of leach liquor decomposes with ilmenite sulfuric acid and the composition of carrying the titanium white waste liquid after titanium is compared, and component is significantly different.The typical composition of titanium white waste liquid is: Sc
2o
323ppm, TiO
27.4 grams per liters, Fe
2o
3(divalence) 33.7 grams per liters, Al
2o
30.46 grams per liter, free sulfuric acid 2.5 ~ 3 mol/L (
nie Li etc., mining metallurgical engineering, 11 (2) 53-57,1991).
Embodiment 3
Preparation raw material liquid: with embodiment 1.
Preparation organic phase: the Primene JM-T extraction agent of getting technical grade is dissolved in sulfonated kerosene, and adds isooctyl alcohol, and now organic phase volume consists of 6 % Primene JM-T-6 % isooctyl alcohol-88% sulfonated kerosenes.
Fractionation extraction: whole extraction process adopts centrifugal extractor to carry out fractionation extraction, extraction progression is 4 grades of extractions, 6 grades of washings, 3 grades of back extractions.Washings is 0.5mol/L sulfuric acid, and anti-stripping agent adopts 1.0 mol/L hydrochloric acid.The throughput ratio of organic phase, stock liquid, washings, anti-stripping agent is 1:8:0.5:0.5.Through the enrichment of this flow process, extraction yield reaches 92%, and total recovery is greater than 80%.
Above to provided by the invention from anatase octahedrite raw ore the method for scandium-enriched be described in detail; having applied specific case herein sets forth principle of the present invention and embodiment; the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof; should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention; can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (9)
1. an enriching method for scandium in anatase octahedrite raw ore, comprises the following steps:
1) anatase octahedrite raw ore is mixed with mineral acid, obtain scandium leach liquor and tailings;
2) extraction agent is mixed with organic solvent and additive, obtain organic phase;
3) use described organic phase to extract scandium leach liquor, obtain the first extraction liquid;
4) with washings, wash after the first extraction liquid, the scandium element of stripping in described the first extraction liquid with anti-stripping agent, obtains thick scandium solution.
2. method according to claim 1, wherein, in anatase octahedrite raw ore, the grade of Scium trioxide is 40 ~ 400ppm.
3. method according to claim 1, wherein, described mineral acid is to be selected from one or more in hydrochloric acid, nitric acid and sulfuric acid, volumetric concentration is 5 ~ 30%; Leach liquor composition is Sc
2o
35 ~ 150ppm, TiO
20.05 ~ 5 grams per liter, Fe
2o
35 ~ 50 grams per liters, free H
+0.2 ~ 8.0 mol/L.
4. method according to claim 1, wherein, described extraction agent is selected from one or more in higly branched chain hexadecyl primary amine (code name N116), heptadecyl-9-amine (code name N179), 19 ~ pentacosyl-(10 ~ 13)-amine (code name N1923), Primene JM-T.
5. method according to claim 1, wherein, described organic solvent is selected from one or more in sulfonated kerosene, dimethylbenzene, hexanaphthene; Described additive is selected from isooctyl alcohol or TBP; In organic phase, the volume ratio of extraction agent, additive and organic solvent is 1 ~ 20:1 ~ 20:60 ~ 98.
6. method according to claim 1, wherein, described washings is hydrochloric acid, nitric acid or sulfuric acid, volumetric concentration is 0.2 ~ 4 mol/L.
7. method according to claim 1, wherein, described anti-stripping agent is hydrochloric acid or nitric acid, volumetric concentration is 0.2 ~ 4 mol/L.
8. method according to claim 1, wherein, described organic phase, stock liquid, washings and anti-stripping agent throughput ratio are 0.5 ~ 1.5:2 ~ 10:0.25 ~ 2:0.25 ~ 2.
9. method according to claim 1, wherein, described extraction progression is 1 ~ 6 grade, washing progression is 1 ~ 6 grade; Reextraction progression is 1 ~ 6 grade.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367620A (en) * | 2016-09-13 | 2017-02-01 | 南昌大学 | Method for extracting and recycling rare earth from low-content rare earth solution with primary amine extracting agent |
| CN106367622A (en) * | 2016-09-13 | 2017-02-01 | 南昌大学 | High-efficient and green ion-absorbed-type rear earth extraction method by adopting aluminum sulfate as leaching agent |
| CN106636686A (en) * | 2016-11-17 | 2017-05-10 | 攀枝花学院 | Method for extracting scandium from artificial rutile leaching mother liquor produced by hydrochloric acid method |
| CN107675000A (en) * | 2017-09-05 | 2018-02-09 | 中国科学院长春应用化学研究所 | Regulate and control heavy rare-earth extraction separating technology extraction equilibrium acidity and the method for extracting series |
| CN110331289A (en) * | 2019-07-02 | 2019-10-15 | 广西大学 | A method of recycling scandium and sodium sulphate from Bayer process red mud |
| CN112458294A (en) * | 2020-11-20 | 2021-03-09 | 河南荣佳钪钒科技有限公司 | Method for recovering vanadium from titanium white waste acid by chlorination process |
| CN113493874A (en) * | 2020-04-08 | 2021-10-12 | 厦门钨业股份有限公司 | Method for purifying high-purity scandium salt |
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| CN106367620A (en) * | 2016-09-13 | 2017-02-01 | 南昌大学 | Method for extracting and recycling rare earth from low-content rare earth solution with primary amine extracting agent |
| CN106367622A (en) * | 2016-09-13 | 2017-02-01 | 南昌大学 | High-efficient and green ion-absorbed-type rear earth extraction method by adopting aluminum sulfate as leaching agent |
| CN106367622B (en) * | 2016-09-13 | 2018-12-07 | 南昌大学 | It is a kind of using aluminum sulfate as the ion adsorption type re efficient green extracting method of leaching agent |
| CN106636686A (en) * | 2016-11-17 | 2017-05-10 | 攀枝花学院 | Method for extracting scandium from artificial rutile leaching mother liquor produced by hydrochloric acid method |
| CN106636686B (en) * | 2016-11-17 | 2018-09-18 | 攀枝花学院 | Hydrochloric acid method produces synthetic rutile and leaches the method for extracting scandium in mother liquor |
| CN107675000A (en) * | 2017-09-05 | 2018-02-09 | 中国科学院长春应用化学研究所 | Regulate and control heavy rare-earth extraction separating technology extraction equilibrium acidity and the method for extracting series |
| CN110331289A (en) * | 2019-07-02 | 2019-10-15 | 广西大学 | A method of recycling scandium and sodium sulphate from Bayer process red mud |
| CN113493874A (en) * | 2020-04-08 | 2021-10-12 | 厦门钨业股份有限公司 | Method for purifying high-purity scandium salt |
| CN113493874B (en) * | 2020-04-08 | 2022-12-13 | 福建省长汀金龙稀土有限公司 | Method for purifying high-purity scandium salt |
| CN112458294A (en) * | 2020-11-20 | 2021-03-09 | 河南荣佳钪钒科技有限公司 | Method for recovering vanadium from titanium white waste acid by chlorination process |
| CN112458294B (en) * | 2020-11-20 | 2023-03-14 | 河南荣佳钪钒科技有限公司 | Method for recovering vanadium from titanium white waste acid produced by chlorination process |
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