Method of producing scandium-bearing concentrate from red mud

IPC classes for russian patent Method of producing scandium-bearing concentrate from red mud (RU 2484164):

C22B59 - Obtaining rare earth metals

C22B3/24 - by adsorption on solid substances, e.g. by extraction with solid resins

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FIELD: metallurgy.

SUBSTANCE: proposed method comprises sulfuric acid leaching of scandium from red mud, pulp filtration, scandium sorption from sulfuric acid solutions, desorption from organic phase by carbonate solution to obtain column effluent. Then, scandium poorly soluble compounds are precipitated from column effluent, precipitate is filtered out, flushed, dried and annealed to get scandium-bearing concentrate. Note here that said leaching is performed by 10.0-13.5%-sulfuric acid at pulp initial vibration cavitation at rotary velocity of 35-60 m/s for 15-35 min. Scandium is precipitated from column effluent by potassium caprinate in amount of 75-100 g/t of scandium at pH 3.5-4.5 and exposure for 15-25 min.

EFFECT: increased yield.

3 cl, 2 tbl, 2 ex

The invention relates to ferrous metallurgy, namely the complex processing of red mud from alumina production.

The method for extracting scandium from the red mud of alumina production based on pyrometallurgical processing thereof and subsequent sulfatization product processing - belitovogo sludge (Derevyankin, VA, Saltanov CENTURIES and other "Improved version providercomcast technology to recycle red mud". - Works YOUR Problem alumina production in the USSR". L.: 1990, p.101). The method includes pyrometallurgical processing of red mud at 1200-1400°C to metalproduct and alumosilicates slag, soda treatment of the latter with receiving belitovogo sludge, sulfatization belitovogo slurry at 200°C for 1 hour and concentrated (90,0%) sulfuric acid, water leaching of sulfate mass at 50°C for 45,0-60 min with a production of scandium-containing sulfuric acid solution, precipitation of scandium from the solution by organic chelating agents (derivatives of polyamines) at a flow rate of precipitating 150-200 g/g Sc, filtering the precipitate, drying and calcining the latest with the receipt of scandium-containing concentrate. The extraction of scandium in the concentrate from the source content in the red sludge is ~65%, and the content in concentrate 10-15 wt.%.

The disadvantages of this method PR is continued to be associated with the complexity and multi-stage technological process of processing of red mud as such, including high-temperature annealing, soda leaching, sulfatization concentrated sulfuric acid and then getting scandium-containing concentrate from the received scandium-containing solution.

This causes also not a high degree of extraction of scandium from the original red mud, and the use of derivatives of polyamines as organic precipitant scandium - low maintenance last in concentrate, because it is quantitative (85-95%) precipitation of iron ions, aluminum, titanium and rare earth elements.

The method for extracting scandium from red mud, including leaching of red mud first 3-5%hydrochloric acid at 20-25°C and the ratio of T:W=1:5-10, then subsequent processing 50-55%sulfuric acid at 100-110°C and T:W=1:6-8 (RF patent No. 2040587, SW 59/00).

Then obtained from scandium-containing sulfuric acid solution of scandium optionally concentrated by known methods by sorption and/or extraction, with subsequent elution of the scandium from the organic phase with sodium carbonate solution, acidification of the solution, precipitation of scandium from a solution of an alkaline reagent, drying and calcining the precipitate to obtain scandium-containing concentrate (Korshunov astray freight, A. M. Reznik and others Scandium. M.: metallurgy, 1987).

This method gidrohimicheskih the recovery of scandium from red mud has several disadvantages. This is primarily a two-stage leaching of red mud, and in the second stage used sulfuric acid of high concentration, which leads to significant recovery of macro - Fe, Al, Ti, whose concentration in the resulting sulfuric acid solution manifold (500-1000 times higher than the concentration of scandium (0.02-0.03 g/DM³); this necessitates 2-3-stage sorption and/or extraction of scandium to obtain sufficiently pure scandium-containing solutions, which not only complicates the technological process, but also reduces end-to-end extraction of scandium from red mud in the concentrate to 65-70%.

The closest to the technological nature, the totality of symptoms and the achieved technical result is a method of obtaining a scandium-containing concentrate of various industrial wastes, including those from red mud from alumina production.

The method consists of the following (patent RF №2048564, SW 59/00).

Is acid leaching of red mud from alumina production solutions of hydrochloric (20-25%HCl) or sulfuric acid (20-30%H₂SO₄), then the slurry is filtered or centrifuged, spend sorption extraction of scandium from the obtained acidic solution, the sorbent is washed for cleaning from a partially sorted impurity ions of aluminum, iron, titanium, implementing tlaut desorption of scandium carbonate-bearing solution with the receipt of the eluate, next, the scandium-containing eluate is treated with mineral acid to a pH of≤1,0, introducing an alkaline reagent to obtain pH values of 1.8 to 2.2, conduct exposure at 60-100°C 15-60 min, separated oxyhydrate precipitate impurities from the solution by filtration, the filtrate precipitated less soluble compounds of scandium, the precipitate was separated by filtration, washed, dried and calcined getting scandium-containing concentrate.

The disadvantages of this method is the relatively low end-to-end extraction of scandium in the target product because of mnogostadiinost process and also low content of scandium in the se product because of the significant transition of the impurity macro when used for leaching of red mud is very concentrated solutions of mineral acids.

The technical result - provision of conditions for increasing the degree of extraction of scandium and the increase in the content of scandium in the target product.

This goal is achieved by a method of obtaining a scandium-containing concentrate from red mud from alumina production, which includes acid leaching of red mud, centrifugation or filtration of the pulp, sorption extraction of scandium from acidic solutions, the washing of the sorbent desorption of scandium carbonate-bearing solution with the receipt of the eluate, the deposition saluate low-solubility compounds of scandium, filtering, washing, drying and calcining the precipitate to obtain scandium-containing concentrate, and differs from the previously known method is the fact that leaching of the red sludge is carried out with solutions of mineral acids and relatively low concentrations in fibroepithelioma mode, and the precipitation of scandium from the received next after sorption-desorption of the eluate spend an organic precipitant - carinatum potassium (K[SN₃(CH₂)₈Soo]) - under certain technological parameters.

The above set of distinctive features provides the technical result consists in increasing the degree of extraction of scandium and the increase of its content in the target product.

Example 1 (the prototype). Is the leaching of red mud from alumina production, containing, wt.%: 46,0 Fe₂O₃, 10,5 Al₂O₃, 9,0 SiO₂, 7,5 CaO, 4,5 TiO₂, 4,0 Na₂O, to 0.011 Sc, 0,035 ZrO₂, 0,05 Y₂O₃, 0,03 GeO₂, 0,03 LaO₅, 0,005 ThO₂- 20%sulfuric acid at 90-95°C, the ratio of W:T=5:1 and the duration of the Next 90 minutes the slurry was filtered, and the obtained scandium-containing solution containing, g/DM³: 55,0 Fe₂O₃, 15,0 Al₂O₃, 1,0 TiO₂, 0,02 Sc, of 0.02 Zr, 0,06 Y₂O₃, 0,05 GeO₂, 0,005 ThO₂, 100 H₂SO_{4 St}- 1,0 DM³PR is leading in contact under dynamic conditions with 10.0 g phosphate material, for example AFI-22 or ANKH-80; sorption was carried out before the appearance of ions in the filtrate scandium (0.002 g/DM³). Further, the ion exchanger was washed with 1.0 N HCl solution in an amount of 0.1 DM³and spent desorption of scandium 3,0 N solution of sodium carbonate (Na₂CO₃in dynamic conditions, passing through the ion exchanger in an amount of 0.1 DM³by getting this eluate (pH 9,5), containing, g/DM³: 0,2 Sc, 0,5 Zr, 1,0 Ti, 0,6 Y₂O₃Of 0,65 Fe, 0,70 Al 0,02 Y, 0,001 Th. The eluate is neutralized to a pH of 0.8, heat the solution to 70°C and incubated for 10 min with stirring. The neutralized solution is alkalinized with an alkaline reagent (NaOH) to a pH of 2.0 and incubated further at 70°C for 45 min with stirring. Fallen oxyhydrate precipitate impurities are separated from the solution by filtration, the filtrate is alkalinized with NaOH solution to pH 6.0 and incubated at 80°C for 90 minutes the precipitation is filtered off, washed, dried and calcined at 750°C for 60 min with a production of scandium-containing concentrate.

Through the extraction of scandium in the target product was:

0,75·0,94·0,96=0,67 or 67.0% (where 75,0, 94,0 and 96,0 - the degree of extraction of scandium, respectively, in the leaching of the red sludge, sorption-desorption and extraction of the eluate in the concentrate), and the content of Sc₂O₃the concentrate was 20.5%.

Example 2. Is acid selachian this red mud under the following process parameters: temperature 90-95°C, the ratio of W:T=5:1, the sulfuric acid concentration of 12.5%, the total duration of leaching 90 min, 25 min early is processed pulp in vibrocavitational the mixer when the value of the peripheral speed of the rotor mixers ω=45 m/sec. Next, the slurry is filtered and the obtained scandium-containing solution containing, g/DM³rating : 10.0 Fe₂O₃, 10,0 Al₂O₃, 0,2 TiO₂, 0,025 Sc, Zr of 0.01, 0.03 to Y₂O₃, 0,001 ThO₂, 40 H₂SO_{4 St}- 1,0 DM³lead contact in dynamic conditions with 10.0 g phosphate material, such as AFI-22 or ANKH-80; sorption was carried out before "breakthrough" (the content of scandium in the filtrate 0.002 g/DM³). Further, the ion exchanger was washed with 1.0 N HCl solution in an amount of 0.1 DM³and spent desorption of scandium 3,0 N solution of sodium carbonate under dynamic conditions in an amount of 0.1 DM³by getting this eluate, containing, g/DM³: 0,3 Sc, 0,1 Zr, 0,12 Ti, 0,25 Fe, 0,40 Al, 0.01 To Y, 0,0003 Th. The eluate was then acidified to pH 4.0, was introduced organic precipitator - caprinate potassium (K[SN₃(CH₂)₈Soo]) in the form of a 0.1 M solution in terms of dosage 85 g of reagent/g of scandium in the solution and held the shutter speed obtained pulp within 20 minutes after the release of sludge was carried out in the laboratory photomachine.

The precipitate was washed on the filter was dried and progulivali at 750°C during 60 min with a production of scandium-containing concentrate.

Through the extraction of scandium in the target product was:

0,80·0,94·0,98=0,737 or 73,7% (where 80,0, 94,0 and 98,0 - the degree of extraction of scandium, respectively, in the leaching of red mud in fibroepithelioma mode, the cycle of sorption-desorption and extraction of the eluate in the concentrate using organic precipitant), and the content of Sc₂O₃in concentrate amounted to 25.0%.

In table 1 and table 2 shows the results of experiments to obtain scandium-containing concentrate from red mud in the implementation process according to the claimed invention, and beyond optimum limits.

Table 1 presents the results for the degree of extraction of scandium and content in the concentrate when the variation of parameters sulfuric acid leaching of red mud under other equal conditions the process as a whole:

leach: temperature 90°C, the ratio of W:T in the original pulp 5:1, the total duration of 90 min;

the deposition of carinatum potassium from the eluate: the value of pH 4.0, the dosage of the organic reagent 85 g/g Sc³⁺extract , 20 minutes

Table 1
The results of the experiments in the implementation process at the optimum mode leaching the Candia ceteris paribus
no experience	The leaching parameters	The degree of extraction of scandium, η, %	The content Sc₂O₃in concentrate, %
C_H2SO4, %	the value of ω, m/s	the vibrating processing time, min
prototype	67,0	20,5
1	10,0	60	15	70,0	23,0
2	12,5	45	25	73,7	25,0
3	13,5	35	35	74,5	22,5
beyond optimum limits
4	8,5	45	25	63,0	21,7
5	15,0	45	25	77,0	16,7
6	12,5	25	25	65,5	20,8
7	12,5	70	25	74,5	18,7
8	12,5	45	10	66,0	21,0
9	12,5	45	45	74,8	18,4
10	8,5	25	10	60,0	22,0
11	13,5	70	45	79,0	of 17.5

Thus, as can be seen from table 1, opt the normal conditions of the sulfuric acid leaching of scandium from red mud, providing ceteris paribus (during the precipitation of scandium from the eluate by carinatum potassium) the achievement of the required technical result is an increase in the degree of extraction of scandium in the concentrate and increase its content in the target product, are as follows (op÷3):

the concentration of sulfuric acid (H₂SO₄) - 10.0 to 13.5 per cent;

- the value of the peripheral speed (ω) of the rotor when fibroepithelioma stirring, m/s - 35-60;

- the duration of the initial vibrocavitational processing sulphate pulp - 15-35 minutes

When you exit the optimum within the parameters of the technological mode leaching:

the decrease in the concentration of sulfuric acid is less than 10% H₂SO₄- there is a decrease in the degree of extraction of scandium to 63.0% (op); the same results in the reduction of the time vibrocavitational processing up to 10 min (op) η_Sc=66,0%, which is less than the required technical result;

- reduce the peripheral speed of the rotor of the mixing device when vibrocavitational processing up to 25 m/sec (op) also leads to a decrease of the degree of extraction of scandium to 65.5%, i.e. less than in the known invention;

- increase one or all three parameters above the upper optimum limit - the concentration of sulfuric acid to 15.0% (op), the values of the peripheral speed of 70 m/s (up) or the length of time the melody is cavitational processing of up to 45 min (op) though and leads to an increase in the degree of extraction of scandium in the concentrate to 74-77%, but significantly reduces its content in the target product to 17.5 to 18.5%. This is due to a simultaneous increase in the extraction of the red mud of elements such as titanium, zirconium, rare earth elements (yttrium, cerium, lanthanum), which together with scandium, partially are sorbed on the phosphate ion and forth seacadets carinatum of potassium carbonate-bearing of the eluate.

Table 2 shows the results on the degree of extraction of scandium and its content in the concentrate when the variation of the deposition parameters of scandium from the eluate under other equal conditions the process as a whole:

leach: the concentration of sulfuric acid (H₂SO₄) - 12.5%, temperature 90°C, the ratio of W:T=5:1, the total duration of 90 min duration vibrocavitational treatment 25 min when the value of the peripheral speed of 45 m/sec.

Table 2
The results of the experiments in the implementation process at the optimum mode of deposition of scandium from the eluate by carinatum potassium
no experience	The deposition parameters	The degree of deposition of the Sc from the eluate	The degree of the extracted what I Sc in the concentrate	The content Sc₂O₃in concentrate, %
dosage org. reagent g/g Sc	pH	the deposition time, min
	prototype	-	67,0	20,5
12	70	3,5	15	92,0	69,0	26,4
13	85	4,0	20	98,0	73,7	25,0
14	100	4,5	25	97,0	72,8	22,0
beyond optimum limits
15	85	3,0	20	84,0	63,0	21,0
16	85	5,0	20	86,0	64,5	19,0
17	60	4,5	20	to 83.5	62,6	22,0
18	110	4,5	20	98,5	74,0	of 17.0
19	85	4,5	10	85,5	64,0	21,0
20	85	4,5	30	98,0	73,5	19,5
21	60	3,0	10	78,0	58,5	18,0
22	110	5,0	30	to 89.5	67,0	16,5

Thus, as can be seen from table 2, the optimal conditions for precipitation of scandium carinatum of potassium obtained after cycle sorption-desorption of the eluate, providing ceteris paribus (with sulfuric acid leaching of scandium from red mud in fibroepithelioma mode) the achievement of the required technical result is an increase in the degree of extraction of scandium in the concentrate and increase its content in the target product, are as follows (op÷14):

- dosage caprinate potassium in an amount of 70-100 g/t scandium in the original solution (eluate);

the pH value of precipitation 3,5÷4,5;

- duration precipitation 15÷25 minutes

When you exit the optimum within the parameters of the technological mode of deposition:

- the output of one or all of the parameters for the lower limit of optimal conditions - reducing the pH of the deposition to 3.0 (op), or dosage caprinate potassium to 60 g/g (op), or deposition time up to 10 min (op) - leads to a significant decrease in precipitation of scandium from the eluate with an organic precipitant, and hence the degree of extraction of scandium from red mud in the concentrate as a whole, respectively, to 83.5-85,5% and up to about 63-64%, which is less than the required technology in the economic result;

- the output of one or all of the parameters for the upper limit of optimal conditions - increasing the pH to 5.0 (op), dosage precipitator to 110 g/g (op) or deposition time of 30 min (op) leads either to reduce the degree of precipitation of scandium from the eluate to 86,0% (op), and hence in the concentrate to 64.5%, or when the positive effect of maintaining the degree of precipitation of scandium from the eluate at the highest possible level 98,0-98,5% (op, 20 and 22) - leads to a significant decrease in the content of scandium in the target the product to ~17-19%, due to the increase in the degree of deposition carinatum potassium passing scandium components of the eluate from carbonate - titanium, zirconium, rare earth elements.

So, only the process of obtaining scandium-containing concentrate from red mud under optimal conditions: leaching of scandium from the red mud of 10.0 to 13.5%sulfuric acid at vibrocavitational initial processing of pulp when the value of the peripheral speed 35-60 m/s for 15-35 min and subsequent precipitation of scandium from received after cycle sorption-desorption of the eluate by carinatum potassium at a dose of 70-100 g/g of scandium at pH 3.5-4.5 and a shutter speed of 15 to 25 minutes is the provision of conditions for increasing the degree of extraction of scandium in the concentrate and the increase of its content in the target product accordingly to ~70,0-75,5% and 22.5-25,0% or higher on CPA is to the known invention (prototype), accordingly 3.0-7.5% and 2.5 to 4.5%.

1. A method of obtaining a scandium-containing concentrate from red mud, including sulfuric acid leaching of scandium from red slurry, filtering the slurry to obtain sulfuric acid solution, sorption of scandium from sulfuric acid solution, washing the adsorbent, desorption of scandium carbonate-bearing solution with the receipt of the eluate, the acidification of the eluate and the precipitation of low-solubility compounds of scandium, filtering the precipitate, washing, drying and calcining the precipitate to obtain scandium-containing concentrate, characterized in that the sulfuric acid leaching initially lead to fibroepithelioma mode, and the precipitation of scandium from the eluate are carinatum potassium.

2. The method according to claim 1, characterized in that the leaching of scandium from red mud are 10,0÷13,5%sulfuric acid initially in fibroepithelioma mode when the value of the peripheral speed 35-60 m/s and duration of 15-35 minutes

3. The method according to claim 1, characterized in that the precipitation of scandium from the obtained eluate by carinatum potassium lead when his dosage 70-100 g/g of scandium when the pH value of 3.5 to 4.5 and a shutter speed of 15-25 minutes