CN115852177A - Method for recycling scandium from fused salt chlorination dust collection slag - Google Patents
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Abstract
The invention discloses a method for recycling scandium from fused salt chlorination dust collection slag, which comprises the following steps: the scandium-rich slag is subjected to high-temperature conversion and fine grinding, and then is leached by sulfuric acid/hydrochloric acid-phosphoric acid to obtain a scandium-rich liquid, a composite extractant is used for countercurrent rotational flow extraction of scandium in the scandium-rich liquid to obtain a loaded organic phase and a raffinate, a mixed solution of hydrogen peroxide, sulfuric acid/hydrochloric acid and phosphoric acid is used for eluting impurities remaining in the loaded organic phase, the alkali liquid is used for carrying out multistage countercurrent rotational flow reverse extraction on the scandium in the eluted loaded organic phase to obtain a scandium hydroxide with the impurity content of less than 1%, and the scandium hydroxide is subjected to hydrochloric acid dissolution, oxalic acid precipitation and high-temperature roasting to finally obtain scandium oxide with the purity of more than 99.9%. The method has the advantages of convenient operation, simple process flow, low production cost, good environmental protection benefit, easy realization of industrialization and high-efficiency recovery of the valuable element scandium in the fused salt chlorination dust-collecting slag.
Description
Technical Field
The invention relates to the technical field of resource recovery, in particular to a method for recovering scandium from molten salt chlorination dust collection slag.
Background
Scandium is an important rare earth element, and oxides and alloys thereof are receiving more and more extensive attention in the fields of aerospace, electric light source materials and clean energy and scarcity thereof. At present, scandium resources mainly exist in sulfuric acid process titanium dioxide waste acid, high titanium slag chlorination link dust collection slag, tungsten slag, red mud in alumina industry and the like, and hydrochloric acid waste liquid in zirconium oxychloride production link and the like. The dust-collecting slag generated in the process of titanium extraction by molten salt chlorination contains a certain valuable element scandium, and the scandium basically exists in the form of soluble salt. Molten salt chlorination and boiling chlorination are two major production methods of titanium tetrachloride, and the titanium tetrachloride produced by the molten salt chlorination accounts for 40 percent of the annual yield of the titanium tetrachloride all over the world. Boiling chlorination has high requirement on the quality of titanium slag raw materials (Ca + Mg is less than 1.0 percent) and has little pollution, while fused salt chlorination has low requirement on the raw materials (also suitable for titanium slag raw materials with high calcium and magnesium), but has heavy pollution, and pollutants such as fused salt chlorination dust-collecting slag discharged in the production process do not have an economical and effective treatment technology at home and abroad, and are treated in a mode of barren stacking or professional slag yard landfill after lime mixing, so valuable scandium resources are wasted.
Therefore, there is a need in the art for an improved process for recovering scandium from molten salt chlorination dust-collecting slag.
Disclosure of Invention
In view of this, an object of the embodiment of the present invention is to provide a method for recovering scandium from molten salt chlorination dust-collecting slag, which is convenient to operate, simple in process flow, low in production cost, good in environmental protection benefit, easy to implement industrialization, and capable of efficiently recovering valuable element scandium from the molten salt chlorination dust-collecting slag.
Based on the above purpose, the embodiment of the invention provides a method for recovering scandium from molten salt chlorination dust-collecting slag, which comprises the following steps:
a. leaching the fused salt chlorination dust-collecting slag to obtain a leaching solution and first leaching residue, washing the first leaching residue to be used as a titanium extraction raw material for recycling, and recycling washing water for leaching the fused salt chlorination dust-collecting slag;
b. precipitating scandium in the leachate by using an alkali liquor containing a strong oxidizing substance to obtain scandium-rich slag and brine, and recovering the brine as a preparation raw material of sodium salt, magnesium salt and calcium salt;
c. after high-temperature conversion and fine grinding, leaching scandium from the scandium-rich slag by using sulfuric acid/hydrochloric acid-phosphoric acid to obtain a scandium-rich solution and a second leaching residue, and recovering the second leaching residue as a manganese extraction and iron-making raw material;
d. performing countercurrent rotational flow extraction on scandium in the scandium-rich liquid by using a composite extractant to obtain a loaded organic phase and raffinate;
e. eluting impurities such as titanium, manganese, calcium, zirconium, iron, magnesium, vanadium and the like remained in the loaded organic phase by using a mixed solution of hydrogen peroxide, sulfuric acid, hydrochloric acid and phosphoric acid, wherein the elution stage number is more than or equal to 1;
f. and (3) carrying out multistage countercurrent rotational flow back extraction on the scandium in the eluted loaded organic phase by using alkali liquor to obtain scandium hydroxide with the impurity content of less than 1%, and dissolving the scandium hydroxide by using hydrochloric acid, precipitating by using oxalic acid, and roasting at high temperature to finally obtain scandium oxide with the purity of more than 99.9%.
In some embodiments, in the step a, the scandium content in the molten salt chlorination dust-collecting slag is 10-150 g/t, and the liquid-solid ratio (volume: mass) in water immersion is (1-10): 1, keeping the pH of the solution to be less than 2 in the leaching process to prevent scandium ions from hydrolyzing and entering solid-phase leaching residues, intensively stirring in the leaching process, keeping the leaching time for 2-5 h to ensure that scandium is fully leached, keeping the pH of water for washing to be less than 2 in the washing process to prevent scandium ions from hydrolyzing, and washing the first leaching residues until the salinity (mass percentage) is less than 0.05%.
In some embodiments, in step b, the alkali liquor is strong oxidizing property, alkaline waste salt water or chlorine alkali chemical tail gas absorption waste liquor generated by purification of molten salt chlorination tail gas, the alkali concentration in the alkali liquor is 5% to 15%, and the alkali liquor and the leaching solution are mixed according to the ratio of (1-1.5): 1, and the reaction time is 1.5 to 3 hours.
In some embodiments, in step c, the scandium-rich slag is subjected to roasting high-temperature conversion at 700-900 ℃, the roasting time is 3-6 h, the scandium-rich slag is converted into oxides after roasting, the roasted product is ground to a particle size range below 250 meshes, and then is leached by sulfuric acid/hydrochloric acid-phosphoric acid, the sulfuric acid concentration is 1-5 mol/L, the hydrochloric acid concentration is 1-5 mol/L, the phosphoric acid concentration is 0.5-2 mol/L, and the leaching time is 2-5 h, so that a scandium-rich solution with low impurity content and a second leaching residue are obtained, wherein the second leaching residue comprises elements such as titanium, manganese, zirconium and iron.
In some embodiments, in step d, the composite extractant comprises, in volume percent: TBP (5-30%), P204 (5-30%), cyanex572 (0-10%) and No. 260 solvent oil (50-90%), wherein the volume ratio of the leachate after the organic phase compound extractant and the water phase are reduced during extraction is 1: (1-30), the extraction equipment is an acid and alkali resistant cyclone extractor, and the extraction stage number is more than or equal to 1.
In some embodiments, in step e, the concentration of sulfuric acid or hydrochloric acid in the mixed solution of hydrogen peroxide-sulfuric acid/hydrochloric acid-phosphoric acid/phosphate is 1-5 mol/L, the concentration of hydrogen peroxide is 1-2 mol/L, the addition amount of phosphoric acid or phosphate is 1-1.5 times of the theoretical amount required for completely removing titanium and zirconium in the organic phase, the elution time is 10-30 min, and the elution number is more than or equal to 1.
In some embodiments, in step f, the alkali solution is a NaOH solution or ammonia water, the concentration is 1.5-3 mol/L, and the volume ratio of the loaded organic phase to the alkali solution in the back extraction is 1: (0.5-2), the back extraction equipment is an acid-alkali-resistant cyclone extractor, the number of back extraction stages is more than or equal to 1, the back extraction product is dissolved by hydrochloric acid to remove silicon-containing impurities, the concentration of the hydrochloric acid is 1-5 mol/L, then scandium ions are precipitated by oxalic acid or sodium oxalate, the addition amount of the oxalic acid or sodium oxalate is 1-1.5 times of the theoretical mass required for completely precipitating the scandium ions, and the precipitate is subjected to centrifugal filtration and dehydration and then is roasted at 600-900 ℃ for 3-6 hours for dehydration and transformation to finally obtain a scandium oxide product with the purity of more than or equal to 99.9%.
The invention has at least the following beneficial technical effects:
the invention provides a method for recovering scandium from fused salt chlorination dust-collecting slag, which is characterized in that impurities in slag are removed and scandium element is purified by carrying out water leaching, alkali liquor leaching, acid liquor leaching, extraction, elution and back extraction on the fused salt chlorination dust-collecting slag for multiple times, and products in the recovery process can be recycled or further applied.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other embodiments can be obtained by using the drawings without creative efforts.
FIG. 1 is a schematic diagram of an embodiment of the method for recovering scandium from the molten salt chlorination dust-collecting slag provided by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
The terms "including" and "having," and any variations thereof, in the description and claims of this invention and the description of the above figures are intended to cover non-exclusive inclusions; the terms "first," "second," and the like in the description and in the claims, or in the drawings, are used for distinguishing between different objects and not necessarily for describing a particular sequential order. The meaning of "plurality" is two or more unless specifically limited otherwise.
Furthermore, reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the invention. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
Fig. 1 shows a method for recovering scandium from molten salt chlorination dust-collecting slag, which comprises the following steps:
a. leaching the fused salt chlorination dust-collecting slag to obtain a leaching solution and first leaching residue, washing the first leaching residue to be used as a titanium extraction raw material for recycling, and recycling washing water for leaching the fused salt chlorination dust-collecting slag;
b. precipitating scandium in the leachate by using an alkali liquor containing a strong oxidizing substance to obtain scandium-rich slag and brine, and recovering the brine as a preparation raw material of sodium salt, magnesium salt and calcium salt;
c. after high-temperature conversion and fine grinding, leaching scandium from the scandium-rich slag by using sulfuric acid/hydrochloric acid-phosphoric acid to obtain a scandium-rich solution and a second leaching residue, and recovering the second leaching residue as a manganese extraction and iron-making raw material;
d. performing countercurrent rotational flow extraction on scandium in the scandium-rich liquid by using a composite extractant to obtain a loaded organic phase and raffinate;
e. eluting impurities such as titanium, manganese, calcium, zirconium, iron, magnesium, vanadium and the like remained in the loaded organic phase by using a mixed solution of hydrogen peroxide, sulfuric acid, hydrochloric acid and phosphoric acid, wherein the elution stage number is more than or equal to 1;
f. and (3) carrying out multistage countercurrent rotational flow back extraction on the scandium in the eluted loaded organic phase by using alkali liquor to obtain scandium hydroxide with the impurity content of less than 1%, and dissolving the scandium hydroxide by using hydrochloric acid, precipitating by using oxalic acid, and roasting at high temperature to finally obtain scandium oxide with the purity of more than 99.9%.
Further, in the step a, the scandium content in the molten salt chlorination dust-collecting slag is 10-150 g/t, and the solid-to-solid ratio (volume: mass) of the water leaching solution (1-10): 1, in the leaching process, the pH of a solution is required to be kept to be less than 2 so as to prevent scandium ions from hydrolyzing and entering solid-phase leaching residues, when the pH does not meet the requirement, acid is properly added to adjust the pH to be less than 2, the leaching process is stirred intensively, the leaching time is 2-5 h so as to ensure that scandium is leached sufficiently, water used for washing is required to be kept to be less than 2 so as to prevent scandium ions from hydrolyzing, washing water can return to the water leaching process, the leaching residues are washed until the salt content (mass percentage) is less than 0.05%, the washed leaching residues can further recover titanium, the washing water can be used for circular washing and can also be used as a leaching agent for next leaching of fused salt chlorination dust collection residues, the washing water is determined according to the amount of the washing water, the washing water in the whole process is not discharged, and the leaching liquid is used as a scandium extraction and reuse raw material.
Further, in step b, the alkali liquor containing the strong oxidizing substance may be strong oxidizing substance, alkaline waste salt water or chlor-alkali chemical tail gas absorption waste liquid generated by purification of molten salt chlorination tail gas, caustic soda may be properly added to ensure that the alkali concentration in the strong oxidizing and strong alkaline solution is 5% -15%, and the alkali liquor and the leaching solution are mixed according to the ratio of (1-1.5): 1, mixing, reacting for 1.5-3 h, and filtering to obtain scandium-rich slag and brine, wherein the brine can be recycled as a raw material for preparing sodium salt, magnesium salt and calcium salt, and the scandium-rich slag is used as a raw material for extracting scandium in the next step.
Further, in the step c, the scandium-rich slag is roasted at 700-900 ℃ for high-temperature conversion, the roasting time is 3-6 h, the roasting is basically converted into oxides, the roasting aims to convert compounds of elements such as iron, manganese, titanium, zirconium and the like into oxides which are insoluble or slightly soluble or slowly soluble in normal-temperature dilute acid so as to be beneficial to the separation of scandium and impurities during the subsequent dilute acid normal-temperature leaching, the roasted products need to be ground to a particle size range below 250 meshes, then the scandium-rich liquid with low impurity content and the leaching residues containing the main impurities such as titanium, manganese, zirconium, iron and the like are obtained by sulfuric acid/hydrochloric acid-phosphoric acid leaching, the sulfuric acid concentration is 1-5 mol/L or the hydrochloric acid is 1-5 mol/L, the phosphoric acid is 0.5-2 mol/L, and the leaching residues can be used as manganese extraction and iron making raw materials for recycling.
Further, in the step d, the composite extracting agent comprises the following components in percentage by volume: TBP (5-30%) + P204 (5-30%) + cyanex572 (0-10%) +260# solvent oil (50-90%), before extraction, a composite extracting agent of an organic phase is not needed to be saponified, acidity increase in the extraction process basically has no influence on extraction of scandium ions but is beneficial to inhibiting extraction of other ions, and the volume ratio of the composite extracting agent of the organic phase to leachate after aqueous phase reduction is 1: (1-30), the extraction equipment is an acid and alkali resistant cyclone extractor, the type and the operation parameters of the cyclone extractor can be adjusted according to the condition of the feed liquid, and the extraction stage number is more than or equal to 1.
Further, in the step e, hydrogen peroxide-sulfuric acid/hydrochloric acid-phosphoric acid/phosphate mixed solution is used for eluting impurities such as titanium, manganese, calcium, zirconium, iron, magnesium, vanadium and the like in the loaded organic phase, the concentration of sulfuric acid or hydrochloric acid is 1-5 mol/L, the concentration of hydrogen peroxide is 1-2 mol/L, the adding amount of phosphoric acid or phosphate is 1-1.5 times of the theoretical amount required for completely removing titanium and zirconium in the organic phase, the elution time is 10-30 min, and the elution grade is more than or equal to 1.
Further, in the step f, the alkali liquor for back extraction can be NaOH solution or ammonia water, the concentration is about 1.5-3 mol/L, and the volume ratio of the loaded organic phase to the alkali liquor during back extraction is 1: (0.5-2), the back extraction equipment is an acid and alkali resistant cyclone extractor (which is beneficial to the separation of back extraction products), the type and the operation parameters of the cyclone extractor can be adjusted according to the condition of the feed liquid, and the back extraction stage number is more than or equal to 1. And (2) carrying out after-treatment on the back extraction product to obtain a scandium oxide product, wherein the after-treatment comprises hydrochloric acid dissolution, oxalic acid precipitation and high-temperature roasting, specifically, the back extraction product is dissolved by hydrochloric acid, the concentration of the hydrochloric acid is 1-5 mol/L, silicon-containing impurities can be removed in the hydrochloric acid dissolution process, scandium ions are precipitated by oxalic acid or sodium oxalate in the scandium-containing impurity removal liquid, the adding amount of the oxalic acid and the sodium oxalate is 1-1.5 times of the theoretical mass required for completely precipitating the scandium ions, and the precipitate is subjected to centrifugal filtration and dehydration and then is roasted at 600-900 ℃ for 3-6 h for dehydration and transformation to finally obtain the scandium oxide product with the purity of more than or equal to 99.9%.
The method for recovering scandium from the molten salt chlorination dust-collecting slag disclosed by the embodiment of the invention is specifically described by taking the molten salt chlorination dust-collecting slag obtained by sampling for a certain time as an example.
Example 1
The main components of the molten salt chlorination dust-collecting slag obtained by sampling are shown in table 1.
Table 1 Main component of fused salt chlorination dust collection slag obtained by sampling
And (2) according to the liquid-solid ratio of 5:1, carrying out water leaching on the fused salt chlorination dust collection slag, wherein the leaching process is carried out under the condition of strong stirring, the leaching time is 4 hours, the leaching rate of scandium is about 90 percent, and a leaching solution is obtained, and the pH value of the leaching solution is about 1.2; precipitating scandium in the leaching solution by using strong oxidizing property and alkaline waste brine generated by purifying the tail gas of molten salt chlorination by adjusting the alkali concentration to 10%, wherein the alkali solution and the leaching solution are mixed in a ratio of 1:1, mixing for 2h, and controlling the pH value at the end of the reaction to be about 7 to ensure that scandium ions are completely precipitated to obtain scandium-rich slag, wherein the scandium ions basically and completely enter the precipitate in the process; carrying out roasting high-temperature conversion on the scandium-rich slag at 750 ℃ for 5h to obtain an oxide after roasting, finely grinding the oxide to a particle size range below 300 meshes, and then leaching for 3h by using a mixed solution of 3mol/L sulfuric acid and 1mol/L phosphoric acid to obtain a scandium-rich solution, wherein the leaching rate of scandium is about 96%, the leaching rate of main impurity elements of titanium is less than 1%, the leaching rate of manganese is less than 2%, the leaching rate of zirconium is less than 1%, and the leaching rate of iron is less than 5%; the scandium in the scandium-rich liquid is directly extracted by counter-current rotational flow under unsaponifiable conditions by using composite extracting agents TBP (5%), P204 (20%), cyanex572 (5%) and No. 260 solvent oil (70%), compared with 1:10, the extraction rate of scandium reaches 99.5%, and the extraction rate of the rest impurities in the scandium-containing solution is only about 0.1-1%, so as to obtain a loaded organic phase and raffinate; eluting impurities remained in the loaded organic phase by using a mixed solution of hydrogen peroxide, sulfuric acid and phosphoric acid, wherein the concentration of sulfuric acid is 4.5mol/L, the concentration of hydrogen peroxide is 1.3mol/L, the adding amount of phosphoric acid is 1.1 times of the theoretical amount required for completely removing titanium and zirconium in the organic phase, the elution time is 20min, the elution number is 3, and the loss rate of scandium in the process is about 0.3%; carrying out multistage countercurrent rotational flow back extraction on the loaded organic phase by using 3mol/L NaOH solution, wherein compared with 1:1, obtaining scandium hydroxide with impurity content less than 1%, wherein the scandium back extraction rate in the process is about 99%; and completely dissolving the scandium hydroxide by hydrochloric acid with the concentration of 1mol/L, and precipitating by sodium oxalate to obtain a precipitate, wherein the addition amount of the sodium oxalate is 1.1 times of the theoretical mass required for completely precipitating scandium ions, and the precipitate is calcined at 850 ℃ for 5 hours after centrifugal filtration and dehydration to finally obtain scandium oxide with the purity of 99.92%.
The foregoing is an exemplary embodiment of the present disclosure, but it should be noted that various changes and modifications could be made herein without departing from the scope of the present disclosure as defined by the appended claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
It should be understood that, as used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly supports the exception. It should also be understood that "and/or" as used herein is meant to include any and all possible combinations of one or more of the associated listed items.
The numbers of the embodiments disclosed in the embodiments of the present invention are merely for description, and do not represent the merits of the embodiments.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements and the like that may be made without departing from the spirit or scope of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (7)
1. A method for recovering scandium from molten salt chlorination dust collection slag is characterized by comprising the following steps:
a. leaching the fused salt chlorination dust collection slag to obtain a leachate and a first leaching residue, wherein the first leaching residue is recycled as a titanium extraction raw material after being washed, and washing water is recycled for leaching the fused salt chlorination dust collection slag;
b. precipitating scandium in the leachate by using an alkali liquor containing a strong oxidizing substance to obtain scandium-rich slag and brine, and recovering the brine as a preparation raw material of sodium salt, magnesium salt and calcium salt;
c. after high-temperature conversion and fine grinding, leaching scandium from the scandium-rich slag by using sulfuric acid/hydrochloric acid-phosphoric acid to obtain a scandium-rich solution and a second leaching residue, wherein the second leaching residue is recovered as a manganese extraction and iron making raw material;
d. performing countercurrent rotational flow extraction on scandium in the scandium-rich liquid by using a composite extractant to obtain a loaded organic phase and raffinate;
e. eluting impurities such as titanium, manganese, calcium, zirconium, iron, magnesium, vanadium and the like remained in the loaded organic phase by using a mixed solution of hydrogen peroxide, sulfuric acid, hydrochloric acid and phosphoric acid, wherein the elution grade number is more than or equal to 1;
f. and (3) carrying out multistage countercurrent rotational flow back extraction on the scandium in the eluted loaded organic phase by using alkali liquor to obtain a scandium hydroxide with the impurity content of less than 1%, and dissolving the scandium hydroxide by using hydrochloric acid, precipitating by using oxalic acid, and roasting at high temperature to finally obtain scandium oxide with the purity of more than 99.9%.
2. The method for recovering scandium from molten salt chlorination dust-collecting slag according to claim 1, wherein in step a, the content of scandium in the molten salt chlorination dust-collecting slag is 10-150 g/t, and the liquid-solid ratio (volume: mass) in water leaching is (1-10): 1, keeping the pH of the solution to be less than 2 in the leaching process to avoid scandium ions from being hydrolyzed into solid-phase leaching residues, strengthening stirring in the leaching process, ensuring that scandium is fully leached, keeping the pH of the solution to be less than 2 in water used for washing in the washing process to prevent scandium ions from being hydrolyzed, and washing the first leaching residues until the salinity (mass percentage) is less than 0.05%.
3. The method for recovering scandium from molten salt chlorination dust-collecting slag according to claim 1, wherein in step b, the alkali liquor is strong oxidizing, alkaline waste brine or chlorine alkali chemical tail gas absorption waste liquor generated by purification of molten salt chlorination tail gas, the alkali concentration in the alkali liquor is 5% -15%, and the alkali liquor and the leachate are mixed according to the ratio of (1-1.5): 1, and the reaction time is 1.5 to 3 hours.
4. The method for recovering scandium from molten salt chlorination dust-collecting slag according to claim 1, wherein in step c, the scandium-rich slag is subjected to roasting high-temperature conversion at 700-900 ℃, the roasting time is 3-6 h, the scandium-rich slag is converted into oxide after roasting, the roasted product is ground to a particle size range below 250 meshes, and then is leached by sulfuric acid/hydrochloric acid-phosphoric acid, the sulfuric acid concentration is 1-5 mol/L, the hydrochloric acid concentration is 1-5 mol/L, the phosphoric acid concentration is 0.5-2 mol/L, and the leaching time is 2-5 h, so that a scandium-rich solution with low impurity content and a second leaching residue are obtained, wherein the second leaching residue comprises elements such as titanium, manganese, zirconium and iron.
5. The method for recovering scandium according to claim 1, wherein in step d, the composite extractant includes, in volume percent: TBP (5-30%), P204 (5-30%), cyanex572 (0-10%) and No. 260 solvent oil (50-90%), wherein the volume ratio of the leachate after the organic phase compound extractant and the water phase are reduced during extraction is 1: (1-30), the extraction equipment is an acid and alkali resistant cyclone extractor, and the extraction stage number is more than or equal to 1.
6. The method for recovering scandium from molten salt chlorination dust-collecting slag according to claim 1, wherein in step e, the concentration of sulfuric acid or hydrochloric acid in the mixed solution of hydrogen peroxide solution-sulfuric acid/hydrochloric acid-phosphoric acid/phosphate is 1-5 mol/L, the concentration of hydrogen peroxide solution is 1-2 mol/L, the addition amount of phosphoric acid or phosphate is 1-1.5 times of the theoretical amount required for completely removing titanium and zirconium in the organic phase, the elution time is 10-30 min, and the elution number is more than or equal to 1.
7. The method for recovering scandium from molten salt chlorination dust-collecting slag according to claim 1, wherein in step f, the alkali liquor is NaOH solution or ammonia water, the concentration is 1.5-3 mol/L, and the volume ratio of the loaded organic phase to the alkali liquor in back extraction is 1: (0.5-2), the back extraction equipment is an acid-alkali-resistant cyclone extractor, the number of back extraction stages is more than or equal to 1, the back extraction product is dissolved by hydrochloric acid to remove silicon-containing impurities, the concentration of the hydrochloric acid is 1-5 mol/L, then scandium ions are precipitated by oxalic acid or sodium oxalate, the addition amount of the oxalic acid or sodium oxalate is 1-1.5 times of the theoretical mass required for completely precipitating the scandium ions, and the precipitate is subjected to centrifugal filtration and dehydration and then is roasted at 600-900 ℃ for 3-6 h for dehydration and transformation to finally obtain a scandium oxide product with the purity of more than or equal to 99.9%.
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| CN117385207A (en) * | 2023-12-11 | 2024-01-12 | 承德宝通矿业有限公司 | Method for recycling scandium in ultra-lean vanadium titano-magnetite iron tailings |
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| CN117385207A (en) * | 2023-12-11 | 2024-01-12 | 承德宝通矿业有限公司 | Method for recycling scandium in ultra-lean vanadium titano-magnetite iron tailings |
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