CN104263926A - Scandium extraction technology of scandium-containing ultra-basic rock - Google Patents
Scandium extraction technology of scandium-containing ultra-basic rock Download PDFInfo
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- CN104263926A CN104263926A CN201410484192.8A CN201410484192A CN104263926A CN 104263926 A CN104263926 A CN 104263926A CN 201410484192 A CN201410484192 A CN 201410484192A CN 104263926 A CN104263926 A CN 104263926A
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Abstract
The invention discloses a scandium extraction technology of a scandium-containing ultra-basic rock. The scandium extraction technology comprises the following steps: 1) ore crushing and grinding, with a scandium-containing ultra-basic rock as a raw ore, crushing the raw ore and feeding to a ball mill, adding water to grind, so as to obtain ore pulp; 2) scandium magnetic separation, namely carrying out magnetic separation on the raw ore; 3) scandium flotation, namely carrying out flotation on magnetic separation tailings; and 4) chemical beneficiation, namely mixing magnetically separated rough scandium concentrate with floated rough scandium concentrate, then carrying out the procedures of roasting, pelletizing, leaching, extracting, pickling, reverse extraction, precipitation, roasting and the like, and finally out scandium metal. The technology disclosed by the invention is reasonable and scientific in steps; aiming at the distribution characteristics of scandium in the ore, magnetic separation, flotation and chemical beneficiation are ingeniously combined, so that the technology has a good separation effect, effective utilization and efficient extraction of the scandium-containing ultra-basic rock are achieved, scandium can be fully recovered, the recovery rate of the scandium is high, the overall process is concise in processing steps, and easy to achieve, the production flow is effectively shortened, and wide popularization and application are facilitated.
Description
Technical field
The invention belongs to and put forward scandium technical field containing scandium ultrabasic rocks, be specifically related to a kind ofly put forward scandium technique containing scandium ultrabasic rocks.
Background technology
Scandium is a kind of softness, argenteous low transition metal, and often exist with the mixing such as gadolinium, erbium, output is little.Scandium is in the low and high dispersing of occurring in nature abundance, and only have 5 grams inside each ton of crust materials, domestic scandium does not almost have self-existent metalliferous mineral, generally composes with isomorphous form and is stored in other mineral, as ilmenite, titanaugite etc.
Due to rare and extract very difficult, the price of scandium is very high, the method of current extraction scandium mainly concentrates on sulfuric acid waste, the chlorination flue dust in titanium production process, the Tailing of titanium separation of producing titanium dioxide and reclaims scandium, domestic production unit has east, Shanghai to rise titanium powder plant, cobalt smeltery, Ganzhou, Guangzhou titanium powder plant etc., its material collection bothers, cost is high, and extraction process is complicated, and scandium extraction yield neither be very desirable.
For this reason, research and develop a kind of technical process succinct, be easy to realize, can from raw ore extracting directly scandium metal, and the technique that scandium extraction yield is high, for when gesture needed for.
Summary of the invention
For above-mentioned deficiency, the object of the invention is, provide a kind of technical process succinct, be easy to realize, and the extraction yield of scandium high put forward scandium technique containing scandium ultrabasic rocks.
For achieving the above object, technical scheme provided by the present invention is:
What contain scandium ultrabasic rocks puies forward a scandium technique, and it comprises the following steps:
(1) broken and ore grinding: to contain scandium ultrabasic rocks for raw ore, will feed in ball mill after crushing raw ore, then add water grinding, obtains the ore pulp that ore particle degree-200 order accounts for 50% ~ 55%; Wherein the mass ratio of water and raw ore is 1: 1.
(2) scandium magnetic separation: carry out magnetic separation to ore pulp, magneticstrength is 6000 ~ 6500 oersteds, obtains containing magnetic separation scandium rough concentrate and the magnetic tailing that scandium oxide grade is 350 ~ 400g/t after magnetic separation.
(3) scandium flotation: carry out flotation to magnetic tailing, obtains the flotation scandium rough concentrate that scandium oxide grade is 350 ~ 400g/t; Described step (3) specifically comprises the following steps: (3.1) carry out flotation to magnetic tailing, and add sulfuric acid 500 ~ 600g/t and adjust mash acid alkalinity to pH=5 ~ 6, MOH 800 ~ 900g/t, stirs 1 ~ 10 minute; (3.2) add No. 2 oil again and make pore forming material 20 ~ 30g/t, stir and open charging valve after 1 ~ 10 minute, scrape bubble 2 ~ 11 minutes, obtain the flotation scandium rough concentrate that scandium oxide grade is 350 ~ 400g/t.
(4) chemical mineral processing: by magnetic separation scandium rough concentrate and the mixing of flotation scandium rough concentrate, then carry out roasting granulation, carry out fluidization wash after cooling, obtain ore particle; Ore particle is leached, obtains filtrate; Secondary cross current solvent extraction is carried out to filtrate, scandium is enriched in extract layer; Level Four cross-flow pickling deironing is adopted to the scandium in extract layer, obtains the scandium after removal of impurities; Back extraction is carried out to the scandium after removal of impurities, forms scandium hydroxide precipitation; By dissolving with hydrochloric acid scandium hydroxide precipitation, and cross the impurity filtering precipitation, obtain scandium solution; In this scandium solution, add oxalic acid scandium is formed precipitation, roasting is carried out to scandium precipitation, the final scandium metal obtaining content 95% ~ 96%.
As a modification of the present invention, described step (4) specifically comprises the following steps:
(4.1) magnetic separation scandium rough concentrate and the mixing of flotation scandium rough concentrate are obtained composite ore, during by composite ore grinding fineness to-0.0385mm content 90% ~ 95%, add Na
2cO
3, carry out roasting granulation, carrying out fluidization wash to wash water pH value after cooling is 7, obtains ore particle;
(4.2) with HCl, ore particle is leached, then filter, obtain filtrate;
(4.3) carry out secondary cross current solvent extraction to filtrate, be enriched in by scandium in extract layer, extraction agent kerosene, extraction phase is than Vo: Va=1: 20;
(4.4) adopt level Four cross-flow pickling deironing to the scandium in extract layer, hydrochloric acid consumption is HCl 5 ~ 6mol/L, compares Vo: Va=1: 1;
(4.5) carry out back extraction to the scandium after removal of impurities, back extraction medicament is NaOH, and consumption is 1.5 ~ 2mol/L, compares Vo: Va=1: 1, and the final scandium hydroxide that formed precipitates;
(4.6) from scandium hydroxide, extract scandium, first by dissolving with hydrochloric acid scandium hydroxide precipitation, then add ammoniacal liquor 4mol/L adjusted to ph to 4.0 ~ 4.5, being heated to more than 100 DEG C to precipitating completely, crossing the impurity filtering precipitation;
(4.7) scandium is formed precipitation, roasting 70 ~ 110 minutes at being deposited in 750 ~ 850 DEG C to scandium by the oxalic acid adding 1mol/L in the scandium solution of removing impurity, the final scandium metal obtaining content 95% ~ 96%.
Beneficial effect of the present invention is: processing step of the present invention is reasonable, science, for scandium distribution character in ore, technique adopts magnetic separation, flotation and chemical mineral processing are multiple ingeniously combines, there is good separating effect, realize effective utilization and the high efficiency extraction to containing scandium ultrabasic rocks, scandium fully can be reclaimed, the scandium rate of recovery is high, can obtain the scandium metal of content 95% ~ 96%, and overall flow processing step is succinct, be easy to realize, effectively shorten Production Flow Chart, be beneficial to wide popularization and application.
Below in conjunction with drawings and Examples, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is mineral processing circuit figure of the present invention.
Embodiment
See Fig. 1, the present embodiment provide a kind of containing scandium ultrabasic rocks put forward scandium technique, it comprises the following steps:
(1) broken and ore grinding: to contain scandium ultrabasic rocks for raw ore, will feed in ball mill after crushing raw ore, then add water grinding, obtain the ore pulp that ore particle degree-200 order accounts for 50% ~ 55%, wherein the mass ratio of water and raw ore is 1: 1;
(2) scandium magnetic separation: magnetic separation is carried out to ore pulp, magneticstrength is 6000 ~ 6500 oersteds, obtains containing magnetic separation scandium rough concentrate and the magnetic tailing that scandium oxide grade is 350 ~ 400g/t after magnetic separation;
(3) scandium flotation: flotation is carried out to magnetic tailing, add sulfuric acid 500 ~ 600g/t and adjust mash acid alkalinity to pH=5 ~ 6, MOH 800 ~ 900g/t, stir 1 ~ 10 minute, add No. 2 oil again and make pore forming material 20 ~ 30g/t, stir and open charging valve after 1 ~ 10 minute, scrape bubble 2 ~ 11 minutes, obtain the flotation scandium rough concentrate that scandium oxide grade is 350 ~ 400g/t;
(4) chemical mineral processing: magnetic separation scandium rough concentrate and the mixing of flotation scandium rough concentrate are obtained composite ore, during by composite ore grinding fineness to-0.0385mm content 90% ~ 95%, adds Na
2cO
3, carry out roasting granulation, maturing temperature is 950 ~ 1000 DEG C, composite ore and Na
2cO
3mass ratio be 5: 1, roasting time is 50 ~ 70 minutes, and carrying out fluidization wash to wash water pH value after cooling is 7, obtain ore particle;
Be that 30%HCl leaches ore particle by mass concentration, leach 1h, then filter at 80 DEG C, obtain filtrate, the mass ratio of its middling particle and HCl is 1: 2;
Carry out secondary cross current solvent extraction to filtrate, extraction agent kerosene, extraction phase is than Vo: Va=1: 20, and extraction time is 6 ~ 15 minutes, is preferably 10 minutes, is enriched in by scandium in extract layer;
Adopt level Four cross-flow pickling deironing to the scandium in extract layer, hydrochloric acid consumption is HCl 5 ~ 6mol/L, compares Vo: Va=1: 1, and washing time is 6 ~ 15 minutes, is preferably 10 minutes;
Carry out back extraction to the scandium after removal of impurities, back extraction medicament is NaOH, and consumption is 1.5 ~ 2mol/L, compares Vo: Va=1: 1, and Stripping times is 6 ~ 15 minutes, is preferably 10 minutes, and the final scandium hydroxide that formed precipitates;
From scandium hydroxide, extract scandium, first by dissolving with hydrochloric acid scandium hydroxide precipitation, then add ammoniacal liquor 4mol/L adjusted to ph to 4.0 ~ 4.5, being heated to more than 100 DEG C to precipitating completely, crossing the impurity filtering precipitation;
Scandium is formed precipitation, roasting 70 ~ 110 minutes at being deposited in 800 DEG C to scandium by the oxalic acid adding 1mol/L in the scandium solution of removing impurity, is preferably 90 minutes, the final scandium metal obtaining content 95% ~ 96%.
In specific implementation process, see following examples.
Raw material is Hebei ultrabasic rocks ore, and its composition percentage composition is scandium 45.65 ~ 78.32g/t.
Raw ore is broken to-50mm through jaw crusher, is then broken to-2mm through roll crusher, feed in ball mill; Add water in the raw ore in described ball mill, water is 1: 1 with the liquid-solid body ratio of raw ore, carries out ore grinding after adding water, and obtains the ore pulp that grinding particle size-0.074mm content accounts for 50 ~ 55%.
The ore pulp of ore grinding gained enters magnetic separation, and magnetic separator field intensity is 6000 ~ 6500 oersteds, obtains contain the magnetic separation scandium rough concentrate that scandium oxide grade is 350 ~ 400g/t, the scandium rate of recovery 37.54% through magnetic separation.
Magnetic tailing enters flotation, add sulfuric acid 500 ~ 600g/t and adjust mash acid alkalinity to pH=5 ~ 6, add collecting agent MOH 800 ~ 900g/t, stir 3 ~ 5 minutes, add No. 2 oil again and make pore forming material 20 ~ 30g/t, stir and open charging valve after 3 ~ 5 minutes, scrape bubble 5 ~ 6 minutes, obtaining scandium oxide grade is 350 ~ 400g/t flotation scandium rough concentrate, the scandium rate of recovery 39.34%.
By magnetic separation scandium rough concentrate and the mixing of flotation scandium rough concentrate, ore grinding, to-0.0385mm content 90% ~ 95%, adds Na
2cO
3, in retort furnace, carry out roasting granulation, maturing temperature is 980 DEG C, and blending ratio is Na
2cO
3: composite ore=0.4, roasting time is 1 hour, and carrying out fluidization wash to wash water pH value after cooling is 7.In the material after washing, add 30%HCl, liquid-solid ratio 2, leach 1 hour at 80 DEG C, cross and filter impurity, obtain filtrate.Carry out secondary cross current solvent extraction to filtrate, extraction agent kerosene, extraction phase is than Vo: Va=1: 20, and extraction time is 10min, is enriched in extract layer by scandium.Adopt level Four cross-flow pickling deironing to the scandium in extract layer, hydrochloric acid consumption is HCl 5 ~ 6mol/L, compares Vo: Va=1: 1, and washing time is 10min.Carry out back extraction to the scandium after deironing, back extraction medicament is NaOH, and consumption is 1.5 ~ 2mol/L, compares Vo: Va=1: 1, effect 10min, and the final scandium hydroxide that formed precipitates.Scandium is extracted from scandium hydroxide, first by dissolving with hydrochloric acid scandium hydroxide precipitation, add ammoniacal liquor 4mol/L adjusted to ph to 4.0 ~ 4.5 again, be heated to more than 100 DEG C to precipitating completely, cross the impurity filtering precipitation, what this process utilized is the otherness that scandium and other impurity metallic elementses precipitate in the basic conditions.Scandium is formed precipitation by oxalic acid again that add 1mol/L in the scandium solution of removing impurity, precipitation is placed in retort furnace, roasting 1.5h at 800 DEG C, the final scandium metal obtaining content 95% ~ 96%, scandium total yield 65.85%.
Above-described embodiment is only the good embodiment of the present invention, and the present invention can not enumerate out whole embodiments, the technical scheme of one of all employing above-described embodiments, or according to the equivalent variations that above-described embodiment does, all in scope.
From above-mentioned, technical process of the present invention is succinct, effectively shortens Production Flow Chart, and there is good separating effect, realize, to the effective utilization and the high efficiency extraction that contain scandium ultrabasic rocks, scandium fully to be reclaimed, the scandium rate of recovery is high, can obtain the scandium metal of content 95% ~ 96%.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change above-mentioned embodiment and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification sheets, these terms just for convenience of description; any restriction is not formed to the present invention; as described in the above embodiment the present invention, step same or similar with it is adopted and other method obtained, all in scope.
Claims (9)
1. what contain scandium ultrabasic rocks puies forward a scandium technique, and it is characterized in that, it comprises the following steps:
(1) broken and ore grinding: to contain scandium ultrabasic rocks for raw ore, will feed in ball mill after crushing raw ore, then add water grinding, obtains the ore pulp that ore particle degree-200 order accounts for 50% ~ 55%;
(2) scandium magnetic separation: magnetic separation is carried out to ore pulp, magneticstrength is 6000 ~ 6500 oersteds, obtains containing magnetic separation scandium rough concentrate and the magnetic tailing that scandium oxide grade is 350 ~ 400g/t after magnetic separation;
(3) scandium flotation: carry out flotation to magnetic tailing, obtains the flotation scandium rough concentrate that scandium oxide grade is 350 ~ 400g/t;
(4) chemical mineral processing: by magnetic separation scandium rough concentrate and the mixing of flotation scandium rough concentrate, then carry out roasting granulation, carry out fluidization wash after cooling, obtain ore particle; Ore particle is leached, obtains filtrate; Secondary cross current solvent extraction is carried out to filtrate, scandium is enriched in extract layer; Level Four cross-flow pickling deironing is adopted to the scandium in extract layer, obtains the scandium after removal of impurities; Back extraction is carried out to the scandium after removal of impurities, forms scandium hydroxide precipitation; By dissolving with hydrochloric acid scandium hydroxide precipitation, and cross the impurity filtering precipitation, obtain scandium solution; In this scandium solution, add oxalic acid scandium is formed precipitation, roasting is carried out to scandium precipitation, final acquisition scandium metal.
2. according to claim 1ly put forward scandium technique containing scandium ultrabasic rocks, it is characterized in that, the mass ratio of water and raw ore is 1: 1 in described step (1).
3. according to claim 1 containing scandium ultrabasic rocks put forward scandium technique, it is characterized in that, described step (3) specifically comprises the following steps:
(3.1) carry out flotation to magnetic tailing, add sulfuric acid 500 ~ 600g/t and adjust mash acid alkalinity to pH=5 ~ 6, MOH 800 ~ 900g/t, stirs 1 ~ 10 minute;
(3.2) add No. 2 oil again and make pore forming material 20 ~ 30g/t, stir and open charging valve after 1 ~ 10 minute, scrape bubble 2 ~ 11 minutes, obtain the flotation scandium rough concentrate that scandium oxide grade is 350 ~ 400g/t.
4. according to claim 1 containing scandium ultrabasic rocks put forward scandium technique, it is characterized in that, described step (4) specifically comprises the following steps:
(4.1) magnetic separation scandium rough concentrate and the mixing of flotation scandium rough concentrate are obtained composite ore, during by composite ore grinding fineness to-0.0385mm content 90% ~ 95%, add Na
2cO
3, carry out roasting granulation, carrying out fluidization wash to wash water pH value after cooling is 7, obtains ore particle;
(4.2) with HCl, ore particle is leached, then filter, obtain filtrate;
(4.3) carry out secondary cross current solvent extraction to filtrate, be enriched in by scandium in extract layer, extraction agent kerosene, extraction phase is than Vo: Va=1: 20;
(4.4) adopt level Four cross-flow pickling deironing to the scandium in extract layer, hydrochloric acid consumption is HCl 5 ~ 6mol/L, compares Vo: Va=1: 1;
(4.5) carry out back extraction to the scandium after removal of impurities, back extraction medicament is NaOH, and consumption is 1.5 ~ 2mol/L, compares Vo: Va=1: 1, and the final scandium hydroxide that formed precipitates;
(4.6) from scandium hydroxide, extract scandium, first by dissolving with hydrochloric acid scandium hydroxide precipitation, then add ammoniacal liquor 4mol/L adjusted to ph to 4.0 ~ 4.5, being heated to more than 100 DEG C to precipitating completely, crossing the impurity filtering precipitation;
(4.7) scandium is formed precipitation, roasting 70 ~ 110 minutes at being deposited in 750 ~ 850 DEG C to scandium by the oxalic acid adding 1mol/L in the scandium solution of removing impurity, the final scandium metal obtaining content 95% ~ 96%.
5. according to claim 4ly put forward scandium technique containing scandium ultrabasic rocks, it is characterized in that, the temperature of roasting is 950 ~ 1000 DEG C in described step (4.1), and roasting time is 50 ~ 70 minutes.
6. according to claim 4 containing scandium ultrabasic rocks put forward scandium technique, it is characterized in that, the mass concentration of the HCl in described step (4.2) is 30%, and the temperature of leaching is 80 DEG C, extraction time is 50 ~ 70 minutes, and the mass ratio of ore particle and HCl is 1: 2.
7. according to claim 4 containing scandium ultrabasic rocks put forward scandium technique, it is characterized in that, the extraction time in described step (4.3) is 6 ~ 15 minutes.
8. according to claim 4 containing scandium ultrabasic rocks put forward scandium technique, it is characterized in that, the washing time in described step (4.4) is 6 ~ 15 minutes.
9. according to claim 4 containing scandium ultrabasic rocks put forward scandium technique, it is characterized in that, the Stripping times in described step (4.5) is 6 ~ 15 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2021055154A (en) * | 2019-09-30 | 2021-04-08 | 住友金属鉱山株式会社 | Method for producing high-purity scandium oxide |
| RU2758439C1 (en) * | 2020-10-22 | 2021-10-28 | Общество с ограниченной ответственностью "Объединенная Компания РУСАЛ Инженерно-технологический центр" | Scandium-containing alumina and its production method |
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Application publication date: 20150107 |