CN103215447A - Method for extracting scandium from scandium-enriched ferrous acid solution by using P204 - Google Patents
Method for extracting scandium from scandium-enriched ferrous acid solution by using P204 Download PDFInfo
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- CN103215447A CN103215447A CN2013101311766A CN201310131176A CN103215447A CN 103215447 A CN103215447 A CN 103215447A CN 2013101311766 A CN2013101311766 A CN 2013101311766A CN 201310131176 A CN201310131176 A CN 201310131176A CN 103215447 A CN103215447 A CN 103215447A
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Abstract
The invention discloses a method for extracting scandium from a scandium-enriched ferrous acid solution by using P204 and belongs to the field of wet metallurgy. The method comprises the step of extracting to remove iron and extracting to extract scandium. The method specifically comprises the following steps: removing iron in the scandium-enriched ferrous acid solution through extraction by using an N235-containing organic phase, wherein the extraction rate is over 99.5 percent, and the scandium loss rate is small than 0.6 percent; and extracting the scandium by using a P204-containing organic phase, wherein the extraction rate is over 99 percent. The scandium content in the scandium-enriched ferrous acid solution is 5-50mg/L, the iron content is 5-45g/L, and the H+ concentration is 1-5.5mol/L. The method is high in scandium recovery rate and low in cost and can meet the requirements of industrial production. The invention provides a novel method for scandium extraction, and the method has wide prospects.
Description
Technical field
The present invention relates to a kind of method, belong to technical field of wet metallurgy with P204 extracting scandium from contain the rich ferrous acid liquid of scandium.
Background technology
Scandium and compound thereof have multiple excellent properties, the adding of scandium has good effect to the performance of improving material, as improvement to alloy, pottery and glass properties, therefore scandium is widely used in high-end technical fields such as national defence, metallurgy, chemical industry, glass, space flight, nuclear technique, laser, electronics, computer, electric light source, superconduction, medical treatment, High-purity Sc Oxide can be used for electronic emission material, superconducting material, solar cell material etc., has high using value.
Scandium belongs to typical dispersed elements, and the abundance in the earth's crust is very low, is about (5～6) * 10
-4%, it is few as the form that independent mineral exist, and has only thortveitite, phosphorus scandium ore deposit and kolbeckite etc. several, therefore is difficult to form independently mineral deposit.
Industrially mainly in handling processes such as tungsten ore, uranium ore, tin ore and ilmenite, reclaim scandium, in addition, in the rare-earth industry, along with the blanking of other composition in the rare-earth mineral, the content of scandium in mine tailing has enrichment significantly, so rare-earth tailing is well to carry the scandium raw material.
The present mine tailing storage in Baogang rare-earth tailing dam is 200,000,000 tons, and speed increment with annual 2000 ten thousand tons, the detection data show, wherein the content of scandium is about 100PPm, being the very high scandium enriched substance of content, is the high quality raw material that extract scandium, extracts the wherein optimum process condition of scandium if can find, realize industrialization, will have very big meaning the output that improves scandium.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defective of prior art, a kind of method with P204 extracting scandium from contain the rich ferrous acid liquid of scandium is provided, problem with scandium extraction difficulty under the high acidity condition on the solution current industrial, the percentage extraction height of the inventive method scandium, cost is low, processing condition are simple and practical, can realize suitability for industrialized production fully.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of method with P204 extracting scandium from contain the rich ferrous acid liquid of scandium, described method comprises the following steps:
(1), extraction deironing:
A) contain the rich ferrous acid liquid of scandium and extract deironing with the organic phase that contains N235, separatory obtains containing scandium water and iron content organic phase, and the weight that contains the organic phase of N235 consists of N235: isooctyl alcohol: kerosene=25:5:70;
2, scandium is carried in extraction:
A) contain the scandium water with the P204 extracting scandium that contains organic phase that consists of P204:TBP: kerosene=25:2:73, obtain containing the scandium organic phase behind the separatory and contain sour water mutually;
B) be that the sodium hydroxide solution of 0.5～4mol/L carries out twice back extraction with the ratio of volume ratio O/W=1:1 to containing scandium organic phase concentration, back extraction obtains the scandium hydroxide precipitation;
C) scandium hydroxide is deposited in 850～1000 ℃ and carried out high temperature sintering 0.5～2 hour, obtain the scandium oxide enriched substance.
Iron content organic phase water, carry out twice back extraction with the ratio of volume ratio O/W=1:1, back extraction obtains highly purified ferric hydroxide precipitate, and the back extraction organic phase is recycled.
The described rich ferrous acid liquid of scandium that contains is obtained with the hydrochloric acid leaching by the Bayan Obo mine tailing, and scandium content is that the content of 5～50mg/L, iron is 5～45g/L, H
+Concentration is 1～5.5mol/L.
The organic phase that contains N235 is volume ratio O/W=1:1 with the ratio that contains the rich ferrous acid liquid of scandium, single extraction.
Among the present invention, P204 is two (2-ethylhexyl phosphoric acids), and N235 is three (suffering-last of the ten Heavenly stems) alkyl tertiary amine, is commonly called as 7301 extraction agents, and TBP is a tributyl phosphate.
Advantage of the present invention is:
The selected process of the present invention is simple, craft science is reasonable, used condition reaches easily, less demanding to reagent and equipment, can from contain the scandium pickling liquor scandium be extracted efficiently, the acid solution behind the deironing collection scandium can reclaim once more to be utilized, and other major impurity element also can effectively be recycled, become Industrial products, the cost in the leaching process of reduction scandium.
Embodiment
Embodiment 1
(1) contain that scandium content is 17mg/L in the rich ferrous acid liquid of scandium, the content of iron is 14.6g/L, H
+Concentration is 3.5mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=25:5:70, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.4%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain scandium water P204 organic extractant phase scandium, the weight of control extracted organic phase consists of P204:TBP: kerosene=25:2:73 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 1.5mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor is filtered, obtain the scandium hydroxide precipitation;
(5) the scandium hydroxide precipitation is carried out calcination, controlled temperature is 900 ℃, and soaking time is 70min, obtains the scandium oxide enriched substance.
Embodiment 2
(1) contain that scandium content is 6mg/L in the rich ferrous acid liquid of scandium, the content of iron is 4.2g/L, H
+Concentration is 1.1mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=28:5:67, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.6%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain scandium water P204 organic extractant phase scandium, the weight of control extracted organic phase consists of P204:TBP: kerosene=23:2:75 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 0.6mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor filtered to get the scandium hydroxide precipitation;
(5) the scandium hydroxide precipitation is carried out calcination, controlled temperature is 850 ℃, and soaking time is 30min, obtains the scandium oxide enriched substance;
Embodiment 3
(1) contain that scandium content is 48mg/L in the rich ferrous acid liquid of scandium, the content of iron is 45.0g/L, H
+Concentration is 5.3mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=20:5:75, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.2%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain the scandium water and extract with the P204 organic phase, the weight of control extracted organic phase consists of P204:TBP: kerosene=22:2:78 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 1.8mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor filtered to obtain high-purity hydrogen Scium trioxide precipitation;
(5) scandium hydroxide is carried out calcination, controlled temperature is 970 ℃, and soaking time is 110min, and gained Scium trioxide purity is 98%, and yield is 90%;
Embodiment 4
(1) contain that scandium content is 19mg/L in the rich ferrous acid liquid of scandium, the content of iron is 15.0g/L, H
+Concentration is 4.1mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=30:5:65, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.7%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain the scandium water and extract with the P204 organic phase, the weight of control extracted organic phase consists of P204:TBP: kerosene=25:2:73 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 2.0mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor filtered to obtain high-purity hydrogen Scium trioxide precipitation;
(5) the scandium hydroxide precipitation is carried out calcination, controlled temperature is 950 ℃, and soaking time is 50min, obtains the scandium oxide enriched substance;
Embodiment 5
(1) contain that scandium content is 16mg/L in the rich ferrous acid liquid of scandium, the content of iron is 13.6g/L, H
+Concentration is 3.1mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=20:5:75, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.4%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain the scandium water and extract with the P204 organic phase, the weight of control extracted organic phase consists of P204:TBP: kerosene=30:2:68 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 2.5mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor filtered to obtain high-purity hydrogen Scium trioxide precipitation;
(5) the scandium hydroxide precipitation is carried out calcination, controlled temperature is 1000 ℃, and soaking time is 60min, obtains the scandium oxide enriched substance;
Embodiment 6
(1) contain that scandium content is 39mg/L in the rich ferrous acid liquid of scandium, the content of iron is 34.6g/L, H
+Concentration is 2.8mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=25:5:70, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.2%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain the scandium water and extract with the P204 organic phase, the weight of control extracted organic phase consists of P204:TBP: kerosene=26:2:72 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 4.0mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor filtered to obtain high-purity hydrogen Scium trioxide precipitation;
(5) the scandium hydroxide precipitation is carried out calcination, controlled temperature is 980 ℃, and soaking time is 60min, obtains the scandium oxide enriched substance;
Embodiment 7
(1) contain that scandium content is 20mg/L in the rich ferrous acid liquid of scandium, the content of iron is 13.6g/L, H
+Concentration is 3.5mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=30:5:65, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.7%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain the scandium water and extract with the P204 organic phase, the weight of control extracted organic phase consists of P204:TBP: kerosene=25:2:73 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 2.0mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor filtered to obtain high-purity hydrogen Scium trioxide precipitation;
(5) the scandium hydroxide precipitation is carried out calcination, controlled temperature is 970 ℃, and soaking time is 60min, obtains the scandium oxide enriched substance;
Embodiment 8
(1) contain that scandium content is 25mg/L in the rich ferrous acid liquid of scandium, the content of iron is 14.8g/L, H
+Concentration is 3.6mol/L, consists of N235 with weight: isooctyl alcohol: the N235 organic extractant phase deironing of kerosene=30:5:65, must contain scandium water and iron content organic phase behind the separatory, and the deironing rate is 99.5%;
(2) iron content organic phase water is carried out back extraction, to be in a ratio of volume ratio O/W=1:1, back extraction twice is filtered water and is got ferric hydroxide precipitate; The back extraction organic phase is recycled.
(3) contain the scandium water and extract with the P204 organic phase, the weight of control extracted organic phase consists of P204:TBP: kerosene=25:2:73 obtains containing the scandium organic phase and contains sour water mutually behind the separatory;
(4) be that the sodium hydroxide solution of 2.0mol/L carries out twice back extraction with volume ratio O/W=1:1 to containing scandium organic phase concentration, the sodium hydroxide strip liquor filtered can obtain high-purity hydrogen Scium trioxide precipitation,
(5) the scandium hydroxide precipitation is carried out calcination, controlled temperature is 920 ℃, and soaking time is 60min, obtains the scandium oxide enriched substance.
It should be noted that at last: obviously, the foregoing description only is for example of the present invention clearly is described, and is not the qualification to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (4)
1. the method with P204 extracting scandium from contain the rich ferrous acid liquid of scandium is characterized in that described method comprises the following steps:
(1), extraction deironing:
A) contain the rich ferrous acid liquid of scandium and extract deironing with the organic phase that contains N235, separatory obtains containing scandium water and iron content organic phase, and the weight that contains the organic phase of N235 consists of N235: isooctyl alcohol: kerosene=25:5:70;
(2), scandium is carried in extraction:
A) contain the scandium water with the P204 extracting scandium that contains organic phase that consists of P204:TBP: kerosene=25:2:73, obtain containing the scandium organic phase behind the separatory and contain sour water mutually;
B) be that the sodium hydroxide solution of 0.5～4mol/L carries out twice back extraction with the ratio of volume ratio O/W=1:1 to containing scandium organic phase concentration, back extraction obtains the scandium hydroxide precipitation;
C) scandium hydroxide is deposited in 850～1000 ℃ and carried out high temperature sintering 0.5～2 hour, obtain the scandium oxide enriched substance.
2. the method with P204 extracting scandium from contain the rich ferrous acid liquid of scandium as claimed in claim 1, it is characterized in that: iron content organic phase water, carry out twice back extraction with the ratio of volume ratio O/W=1:1, back extraction obtains highly purified ferric hydroxide precipitate, and the back extraction organic phase is recycled.
3. the method with P204 extracting scandium from contain the rich ferrous acid liquid of scandium as claimed in claim 1 or 2 is characterized in that: the described rich ferrous acid liquid of scandium that contains is obtained with the hydrochloric acid leaching by the Bayan Obo mine tailing, and scandium content is that the content of 5～50mg/L, iron is 5～45g/L, H
+Concentration is 1～5.5mol/L.
4. the method with P204 extracting scandium from contain the rich ferrous acid liquid of scandium as claimed in claim 3 is characterized in that: the organic phase that contains N235 is volume ratio O/W=1:1 with the ratio that contains the rich ferrous acid liquid of scandium, single extraction.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103667748A (en) * | 2013-12-30 | 2014-03-26 | 贵州鑫亚矿业有限公司 | Method for preparing purified scandium from crude scandium enriched in raw anatase and serving as raw material |
| CN103695671A (en) * | 2014-01-13 | 2014-04-02 | 江西泛美亚材料有限公司 | Method for recycling and purifying scandium oxide powder from waste acid in zirconium salt production |
| CN103741175A (en) * | 2013-12-26 | 2014-04-23 | 广西科技大学 | Method for separating ferrous ions in stannous solution |
| CN103741176A (en) * | 2013-12-26 | 2014-04-23 | 广西科技大学 | Method for separating ferrous ions in stannous solution |
| CN103741174A (en) * | 2013-12-26 | 2014-04-23 | 广西科技大学 | Method for separating ferrous ions in stannous solution |
| CN103757668A (en) * | 2013-12-26 | 2014-04-30 | 广西科技大学 | Method for separating ferrous ion in tin-containing liquid |
| CN106119555A (en) * | 2016-06-23 | 2016-11-16 | 中国神华能源股份有限公司 | A kind of method extracting scandium from flyash |
| CN106916949A (en) * | 2017-03-23 | 2017-07-04 | 南昌航空大学 | The technique of P204 extractions Extraction of rare earth from southern RE ore |
| CN108754156A (en) * | 2018-07-09 | 2018-11-06 | 中南大学 | A kind of method of iron and scandium in extraction separating red mud acid leaching liquor |
| CN110844963A (en) * | 2019-11-21 | 2020-02-28 | 神华准能资源综合开发有限公司 | Method for separating and recovering aluminum-containing high-iron-salt-acid wastewater |
| CN110878389A (en) * | 2019-11-04 | 2020-03-13 | 江西晶安高科技股份有限公司 | Method for treating crystallization mother liquor in zirconium oxychloride production process |
| CN112429780A (en) * | 2020-12-14 | 2021-03-02 | 河南荣佳钪钒科技有限公司 | Method for recovering valuable elements by sectional extraction of titanium white waste acid by chlorination process |
| CN113308603A (en) * | 2021-05-26 | 2021-08-27 | 广西银亿新材料有限公司 | Treatment method of interphase dirt in nickel-cobalt metallurgy P204 extraction system |
| CN115418485A (en) * | 2022-09-15 | 2022-12-02 | 先导薄膜材料（广东）有限公司 | Method for recycling scandium oxide from scandium-containing loaded organic phase |
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| CN103741176B (en) * | 2013-12-26 | 2016-07-13 | 广西科技大学 | Separate the method containing tin liquor ferrous ions |
| CN103741176A (en) * | 2013-12-26 | 2014-04-23 | 广西科技大学 | Method for separating ferrous ions in stannous solution |
| CN103741174A (en) * | 2013-12-26 | 2014-04-23 | 广西科技大学 | Method for separating ferrous ions in stannous solution |
| CN103757668A (en) * | 2013-12-26 | 2014-04-30 | 广西科技大学 | Method for separating ferrous ion in tin-containing liquid |
| CN103741175A (en) * | 2013-12-26 | 2014-04-23 | 广西科技大学 | Method for separating ferrous ions in stannous solution |
| CN103741174B (en) * | 2013-12-26 | 2016-06-08 | 广西科技大学 | Separate the method containing tin liquor ferrous ions |
| CN103741175B (en) * | 2013-12-26 | 2016-07-13 | 广西科技大学 | Separate the method containing tin liquor ferrous ions |
| CN103667748A (en) * | 2013-12-30 | 2014-03-26 | 贵州鑫亚矿业有限公司 | Method for preparing purified scandium from crude scandium enriched in raw anatase and serving as raw material |
| CN103695671B (en) * | 2014-01-13 | 2016-01-27 | 江西赛瓷材料有限公司 | Reclaim in a kind of spent acid by producing zirconates, the method for purification Scium trioxide powder |
| CN103695671A (en) * | 2014-01-13 | 2014-04-02 | 江西泛美亚材料有限公司 | Method for recycling and purifying scandium oxide powder from waste acid in zirconium salt production |
| CN106119555A (en) * | 2016-06-23 | 2016-11-16 | 中国神华能源股份有限公司 | A kind of method extracting scandium from flyash |
| CN106119555B (en) * | 2016-06-23 | 2018-10-12 | 中国神华能源股份有限公司 | A method of extracting scandium from flyash |
| CN106916949A (en) * | 2017-03-23 | 2017-07-04 | 南昌航空大学 | The technique of P204 extractions Extraction of rare earth from southern RE ore |
| CN108754156A (en) * | 2018-07-09 | 2018-11-06 | 中南大学 | A kind of method of iron and scandium in extraction separating red mud acid leaching liquor |
| CN110878389A (en) * | 2019-11-04 | 2020-03-13 | 江西晶安高科技股份有限公司 | Method for treating crystallization mother liquor in zirconium oxychloride production process |
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| CN115418485A (en) * | 2022-09-15 | 2022-12-02 | 先导薄膜材料（广东）有限公司 | Method for recycling scandium oxide from scandium-containing loaded organic phase |
| CN115418485B (en) * | 2022-09-15 | 2024-04-05 | 先导薄膜材料（广东）有限公司 | Method for recovering scandium oxide from scandium-containing loaded organic phase |
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