CN112981146A - Method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting - Google Patents
Method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention discloses a method for recovering rare earth molten salt electrolytic slag by fluorine fixation transformation roasting, which comprises the following steps: 1) mixing fluorine-containing rare earth fused salt electrolysis slag with an additive to obtain a mixture; 2) carrying out fluorine-fixing transformation roasting on the mixture to obtain roasted sand; 3) acid leaching the calcine to obtain a rare earth leaching solution and leaching residues; wherein the additive comprises calcium oxide and calcium chloride. The method provided by the invention realizes ore phase transformation and efficient extraction of rare earth components in the rare earth molten salt electrolytic slag, realizes separation of rare earth and fluorine through fluorine-fixing transformation roasting, inhibits escape of fluorine in the rare earth extraction process, and has the advantages of high rare earth extraction rate, environmental friendliness, simple process and the like.
Description
Technical Field
The invention belongs to the field of metallurgical waste residue treatment and resource utilization, and relates to a method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting.
Background
The main methods for preparing rare earth metal at present are metallothermic reduction method and molten salt electrolysis method. Common rare earth metals such as La, Ce, Pr, Nd and the like are obtained by fluoride system molten salt electrolysis. According to estimation, more than 5% of waste residues generated in the molten salt electrolysis process contain 20-70% of rare earth, exist mainly in the form of fluoride, and are oxyfluoride and oxide, and the waste residues contain a certain amount of elements such as lithium, iron, silicon, carbon and the like, have complex components and have considerable recovery value. At present, the regeneration and recycling technology of rare earth electrolysis waste residues is not mature, the waste residues are discarded as industrial waste or are doped into qualified molten salt for continuous use, but the quality of rare earth products is influenced by the waste residue doping. The currently reported methods for recycling the rare earth molten salt electrolysis slag mainly comprise an acid method and an alkali method.
Chinese patent CN 104805292A adopts low-concentration hydrochloric acid to leach rare earth praseodymium-neodymium fused salt electrolytic slag to obtain filter residue containing praseodymium-neodymium fluoride and filtrate containing praseodymium-neodymium chloride. Only part of rare earth elements can be recovered by adopting the method, and because the impurities such as silicon dioxide, graphite and the like in the molten salt slag are difficult to remove in an acid leaching mode, the acid leaching filter slag is difficult to directly utilize because of containing the impurities.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for recovering rare earth molten salt electrolytic slag by fluorine fixation transformation roasting. By adding the additive for roasting transformation, fluorine in the rare earth fluoride is transformed into more stable fluoride, so that the separation of rare earth elements and fluorine is realized, and the recovery of rare earth is facilitated.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for recovering rare earth molten salt electrolytic slag by fluorine fixation transformation roasting, which comprises the following steps:
(1) mixing fluorine-containing rare earth fused salt electrolysis slag with an additive to obtain a mixture;
(2) carrying out fluorine-fixing transformation roasting on the mixture to obtain roasted sand;
(3) acid leaching the calcine to obtain a rare earth leaching solution and leaching residues;
wherein the additive comprises calcium oxide and calcium chloride.
The treatment object of the invention is waste residue generated by rare earth molten salt electrolysis, which is generally generated by producing single rare earth metal or rare earth alloy by fluoride molten salt electrolysis, and the rare earth in the waste residue mainly exists in the form of fluoride. According to the method, calcium oxide and calcium chloride are compounded in the additive, the calcium oxide mainly plays a role in fluorine fixation and transformation, the calcium chloride is used as an auxiliary agent, and the calcium chloride and the auxiliary agent can better decompose and transform rare earth fluoride into rare earth oxide under the synergistic effect, so that the rare earth oxide and the stable insoluble calcium fluoride are obtained.
The method realizes the mineral phase transformation and the high-efficiency extraction of the rare earth components in the rare earth molten salt electrolytic slag, realizes the separation of rare earth and fluorine through the solid fluorine transformation roasting, inhibits the escape of fluorine in the rare earth extraction process, and has the advantages of high rare earth metal extraction rate, environmental friendliness, simple process and the like.
The source of the fluorine-containing rare earth molten salt electrolytic slag is not limited, and the fluorine-containing rare earth molten salt electrolytic slag can comprise: the waste residue generated by single rare earth metal or rare earth alloy is prepared by adopting a fluoride molten salt electrolysis method. The single rare earth metal may be, for example, praseodymium or neodymium, and the rare earth alloy may be, for example, praseodymium-neodymium alloy.
In a preferred embodiment of the method of the present invention, in the fluorine-containing rare earth molten salt electrolysis slag in step (1), the mass content of the rare earth element is 20% to 70% (e.g., 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, or 70%), the mass content of the fluorine element is 2% to 20% (e.g., 2%, 3%, 5%, 8%, 12%, 15%, or 20%), and the rare earth element is mainly present in the form of fluoride.
Preferably, the fluorine-containing rare earth molten salt electrolysis slag is finely ground before the step (1) until the particle size of the product is less than 100 meshes, such as 120 meshes, 125 meshes, 140 meshes, 160 meshes, 200 meshes or 240 meshes.
Preferably, the amount of the calcium oxide used in the step (1) is 20 to 50% of the fluorine-containing rare earth molten salt electrolysis slag, for example, 20%, 25%, 30%, 35%, 40%, 45%, 50%, and the like, and preferably 25% to 40%.
Preferably, the amount of the calcium chloride used in the step (1) is 10 to 50% of the fluorine-containing rare earth molten salt electrolysis slag, for example, 10%, 20%, 30%, 35%, 40%, or 50%, preferably 10 to 20%.
Preferably, the mass ratio of the calcium oxide to the calcium chloride in the step (1) is (1.5-3): 1, such as 1.5:1, 1.8:1, 2:1, 2.5:1 or 3: 1. The lower mass ratio of calcium oxide to calcium chloride leads to a lower recovery rate of rare earth, and the higher mass ratio of calcium oxide to calcium chloride leads to an increase in temperature required for calcination transformation.
Preferably, the temperature of the fluorine-fixing transformation roasting in the step (2) is 600-1000 ℃, such as 600 ℃, 700 ℃, 750 ℃, 800 ℃, 900 ℃ or 1000 ℃, preferably 750-900 ℃.
Preferably, the time for the fluorine-fixing transformation roasting in the step (2) is 0.5-3 h, such as 0.5h, 1h, 1.5h, 2h, 2.5h or 3 h.
Preferably, the calcine is finely ground after step (2) and before step (3) until the particle size of the product is smaller than 100 meshes, such as 120 meshes, 125 meshes, 140 meshes, 160 meshes, 200 meshes, 240 meshes and the like.
Preferably, the temperature of the acid leaching in the step (3) is 20 to 90 ℃, such as 20 ℃, 25 ℃, 28 ℃, 30 ℃, 35 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃ or 90 ℃ and the like.
Preferably, the acid leaching time in the step (3) is 1-3 h, such as 1h, 1.5h, 2h, 2.5h or 3 h.
Preferably, the liquid-solid ratio of the acid leaching in the step (3) is (5-15): 1, such as 5:1, 6:1, 8:1, 10:1, 12:1, 13:1 or 15: 1.
Preferably, the acid solution used in the acid leaching in the step (3) comprises at least one of hydrochloric acid and sulfuric acid.
Preferably, the concentration of the acid solution is 0.5-3 mol/L, such as 0.5mol/L, 1mol/L, 1.2mol/L, 1.5mol/L, 1.8mol/L, 2mol/L, 2.5mol/L or 3 mol/L.
As a further preferred technical solution of the method of the present invention, the method comprises the steps of:
(1) finely grinding the fluorine-containing rare earth fused salt electrolysis slag until the particle size of the fused salt slag fine material is less than 100 meshes;
(2) adding an additive into the molten salt slag fine material obtained in the step (1), mixing, and then carrying out fluorine fixation transformation roasting to obtain calcine, wherein the additive is a mixture of calcium oxide and calcium chloride, the dosage of the calcium oxide is 25% -40% of the fluorine-containing rare earth molten salt electrolytic slag by mass, and the dosage of the calcium chloride is 10% -20% of the fluorine-containing rare earth molten salt electrolytic slag by mass;
(3) finely grinding the calcine obtained in the step (2) until the particle size of the calcine fine material is smaller than 100 meshes;
(4) and (4) acid leaching the calcine fine material obtained in the step (3) to obtain rare earth leachate and leaching residue.
Compared with the prior art, the invention has the following beneficial effects:
the method provided by the invention realizes effective separation and extraction of rare earth elements in fluorine-containing rare earth fused salt electrolysis slag, and has the advantages of high metal extraction rate, environmental friendliness, simple process and the like. Meanwhile, fluorine elements in the rare earth molten salt slag are separated from rare earth and are converted into more stable fluoride (calcium fluoride) through fluorine-fixing roasting, so that the adverse effect of the rare earth extraction process on the environment is obviously reduced.
Drawings
FIG. 1 is an XRD spectrum of a raw material rare earth molten salt electrolytic slag used in example 1.
FIG. 2 is an XRD pattern of the acid-leached residue in example 1.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The embodiment of the invention provides a method for recovering rare earth molten salt electrolytic slag by fluorine fixation transformation roasting. The method specifically comprises the steps of fine grinding, fluorine fixation roasting, calcine fine grinding, acid leaching and rare earth extraction and the like of the raw material rare earth molten salt electrolytic slag, and exemplarily provides the following embodiments.
Example 1
The embodiment provides a method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting, which comprises the following steps:
(1) 100g of rare earth molten salt electrolysis slag is rod-ground to have the grain diameter of less than 100 meshes, wherein the content of rare earth in the rare earth molten salt electrolysis slag is respectively Nd 52.2 wt% and Pr 2.60 wt%, and the main phases of the rare earth molten salt electrolysis slag are neodymium fluoride and neodymium oxide and contain a small amount of neodymium ferrite (the XRD pattern of the raw material is shown in figure 1).
(2) And (2) mixing the molten salt slag fine material obtained in the step (1) with an additive, wherein the additive is a mixture of calcium oxide and calcium chloride, the dosage of the calcium oxide is 30g, and the dosage of the calcium chloride is 20g, and then carrying out fluorine-fixing transformation roasting to obtain roasted sand. Wherein the temperature of the fluorine-fixing roasting is 800 ℃, and the roasting time is 1 h.
(3) And (3) grinding the roasted product obtained by fluorine fixation roasting in the step (2) to a particle size of less than 100 meshes.
(4) Leaching the roasted fine material obtained in the step (3) by using sulfuric acid, wherein the acid leaching temperature is 80 ℃, the liquid-solid ratio of acid leaching is 10:1, the acid concentration is 1.5mol/L, and the acid leaching time is 2h, so as to obtain rare earth leachate and leaching residue (the main components are calcium sulfate and calcium fluoride, and the XRD (X-ray diffraction) pattern of the leaching residue is shown in figure 2).
In this example, the rare earth extraction rate was 95.2%.
Example 2
The embodiment provides a method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting, which comprises the following steps:
(1) 100g of rare earth molten salt electrolysis slag is rod-milled to have the grain diameter of less than 200 meshes, wherein the raw material components of the rare earth molten salt electrolysis slag are the same as those in example 1.
(2) And (2) mixing the molten salt slag fine material obtained in the step (1) with an additive, wherein the additive is a mixture of calcium oxide and calcium chloride, the dosage of the calcium oxide is 35g, and the dosage of the calcium chloride is 15g, and then carrying out fluorine-fixing transformation roasting to obtain roasted sand. Wherein the temperature of the fluorine-fixing roasting is 900 ℃, and the roasting time is 1 h.
(3) And (3) grinding the roasted product obtained by fluorine fixation roasting in the step (2) to a particle size of less than 200 meshes.
(4) Leaching the roasted fine material in the step (3) by using hydrochloric acid, wherein the acid leaching temperature is 80 ℃, the liquid-solid ratio of acid leaching is 10:1, the acid concentration is 3mol/L, and the acid leaching time is 2h to obtain rare earth leachate and leaching residue (the main component of calcium fluoride).
In this example, the rare earth extraction rate was 96.8%.
Example 3
The embodiment provides a method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting, which comprises the following steps: (1) 100g of rare earth molten salt electrolysis slag is rod-milled to have the grain diameter of less than 200 meshes, wherein the raw material components of the rare earth molten salt electrolysis slag are the same as those in example 1.
(2) And (2) mixing the molten salt slag fine material obtained in the step (1) with an additive, wherein the additive is a mixture of calcium oxide and calcium chloride, the dosage of the calcium oxide is 35g, and the dosage of the calcium chloride is 15g, and then carrying out fluorine-fixing transformation roasting to obtain roasted sand. Wherein the temperature of the fluorine-fixing roasting is 950 ℃, and the roasting time is 1 h.
(3) And (3) grinding the roasted product obtained by fluorine fixation roasting in the step (2) to a particle size of less than 200 meshes.
(4) Leaching the roasted fine material in the step (3) by hydrochloric acid, wherein the acid leaching temperature is 90 ℃, the liquid-solid ratio of acid leaching is 15:1, the acid concentration is 3mol/L, and the acid leaching time is 2h to obtain rare earth leachate and leaching residue (main component calcium fluoride).
In this example, the rare earth extraction rate was 98.3%.
Example 4
The difference from example 1 is that calcium oxide was used in an amount of 15g and calcium chloride was used in an amount of 35 g. The extraction rate of rare earth is 72.7%.
Example 5
The difference from example 1 is that calcium oxide was used in an amount of 45g and calcium chloride was used in an amount of 5 g. In order to achieve the same rare earth extraction rate, the required roasting temperature is 850 ℃.
Comparative example 1
The difference from example 1 is that the additive was 50g of calcium oxide. In order to achieve the same rare earth extraction rate, the required roasting temperature is 950 ℃.
Comparative example 2
The difference from example 1 is that the additive is 50g of calcium chloride. The extraction rate of rare earth is 63.5%.
As can be seen from the comparison between the embodiment 1 and the embodiments 4-5 and the comparison between the embodiment 1 and the comparative examples 2, the additive is a compound of calcium oxide and calcium chloride, which has an important influence on the process of solid fluorine transformation roasting, and the higher rare earth extraction rate can be obtained under the condition of low energy consumption by optimizing the proportion of the calcium oxide to the calcium chloride.
Comparative example 3
The difference from example 1 is that the additive is 50g of sodium hydroxide.
In the process of alkali roasting, fluorine is converted into soluble sodium fluoride, and in addition, the alkali residue in the alkali roasting product is more, so that a large amount of water is needed for washing, and the washing aims to remove the sodium fluoride to separate the sodium fluoride from the rare earth on one hand, remove the residual alkali in the roasting product on the other hand, and reduce the acid consumption of acid leaching of the rare earth. Moreover, the washing process needs higher liquid-solid ratio and more times to completely remove the sodium fluoride and the residual alkali, so that the rare earth extraction process is too long, and a large amount of fluorine-containing wastewater is generated. In addition, soluble sodium silicates and sodium fluorides formed during the alkaline calcination process are prone to filtration difficulties.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (9)
1. A method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting is characterized by comprising the following steps:
(1) mixing fluorine-containing rare earth fused salt electrolysis slag with an additive to obtain a mixture;
(2) carrying out fluorine-fixing transformation roasting on the mixture to obtain roasted sand;
(3) acid leaching the calcine to obtain a rare earth leaching solution and leaching residues;
wherein the additive comprises calcium oxide and calcium chloride.
2. The method according to claim 1, wherein the fluorine-containing rare earth molten salt electrolytic slag of step (1) comprises: the waste residue generated by single rare earth metal or rare earth alloy is prepared by adopting a fluoride molten salt electrolysis method.
3. The method according to claim 1 or 2, wherein in the fluorine-containing rare earth molten salt electrolysis slag obtained in the step (1), the mass content of rare earth elements is 20-70%, the mass content of fluorine elements is 2-20%, and the rare earth elements are mainly in the form of fluorides.
4. The method according to any one of claims 1 to 3, wherein the fluorine-containing rare earth molten salt electrolysis slag is finely ground to a particle size of less than 100 meshes before the step (1).
5. The method according to any one of claims 1 to 4, wherein the calcium oxide in the step (1) is used in an amount of 20 to 50 percent, preferably 25 to 40 percent, by mass of the fluorine-containing rare earth molten salt electrolysis slag;
preferably, the amount of the calcium chloride used in the step (1) is 10-50% of the fluorine-containing rare earth molten salt electrolysis slag by mass, and preferably 10-20%;
preferably, the mass ratio of the calcium oxide to the calcium chloride in the step (1) is (1.5-3): 1.
6. The method according to any one of claims 1 to 5, wherein the temperature of the fluorine-fixing transformation roasting in the step (2) is 600 to 1000 ℃, preferably 750 to 900 ℃;
preferably, the time for the fluorine-fixing transformation roasting in the step (2) is 0.5-3 h.
7. The process according to any one of claims 1 to 6, wherein the calcine is finely ground after step (2) and before step (3) to a particle size of less than 100 mesh.
8. The method according to any one of claims 1 to 7, wherein the temperature of the acid leaching in the step (3) is 20 to 90 ℃;
preferably, the acid leaching time in the step (3) is 1-3 h;
preferably, the liquid-solid ratio of the acid leaching in the step (3) is (5-15): 1;
preferably, the acid solution used in the acid leaching in the step (3) comprises at least one of hydrochloric acid and sulfuric acid;
preferably, the concentration of the acid solution is 0.5-3 mol/L.
9. Method according to any of claims 1-8, characterized in that the method comprises the steps of:
(1) finely grinding the fluorine-containing rare earth fused salt electrolysis slag until the particle size of the fused salt slag fine material is less than 100 meshes;
(2) adding an additive into the molten salt slag fine material obtained in the step (1), mixing, and then carrying out fluorine fixation transformation roasting to obtain calcine, wherein the additive is a mixture of calcium oxide and calcium chloride, the dosage of the calcium oxide is 25% -40% of the fluorine-containing rare earth molten salt electrolytic slag by mass, and the dosage of the calcium chloride is 10% -20% of the fluorine-containing rare earth molten salt electrolytic slag by mass;
(3) finely grinding the calcine obtained in the step (2) until the particle size of the calcine fine material is smaller than 100 meshes;
(4) and (4) acid leaching the calcine fine material obtained in the step (3) to obtain rare earth leachate and leaching residue.
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| CN114703384A (en) * | 2022-03-31 | 2022-07-05 | 江苏南方永磁科技有限公司 | Slag remover material for rare earth recovery and preparation and use methods thereof |
| CN114703384B (en) * | 2022-03-31 | 2023-07-25 | 江苏南方永磁科技有限公司 | Slag remover material for rare earth recovery and preparation and use methods thereof |
| CN114956146A (en) * | 2022-06-02 | 2022-08-30 | 中南大学 | Pretreatment method of fluorine-containing waste residue and recovery method of calcium fluoride |
| CN114956146B (en) * | 2022-06-02 | 2023-08-11 | 中南大学 | Pretreatment method of fluorine-containing waste residues and recovery method of calcium fluoride |
| CN116377258A (en) * | 2023-04-13 | 2023-07-04 | 中国科学院过程工程研究所 | Method for strengthening leaching of rare earth molten salt electrolytic slag |
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Application publication date: 20210618 |