CN113604686A - Precipitation method of aluminum-containing rare earth feed liquid - Google Patents
Precipitation method of aluminum-containing rare earth feed liquid Download PDFInfo
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- CN113604686A CN113604686A CN202110705546.7A CN202110705546A CN113604686A CN 113604686 A CN113604686 A CN 113604686A CN 202110705546 A CN202110705546 A CN 202110705546A CN 113604686 A CN113604686 A CN 113604686A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B59/00—Obtaining rare earth metals
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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Abstract
A precipitation method of an aluminum-containing rare earth feed liquid comprises the following steps: (1) taking the aluminum-containing rare earth feed liquid flowing out of the extraction tank, adding water into the aluminum-containing rare earth feed liquid for dilution, diluting the aluminum-containing rare earth feed liquid to 80g/L, adding an aluminum complexing agent, and uniformly stirring to obtain a mixed solution; (2) adding a precipitator into the mixed solution for precipitation, wherein the precipitation temperature is 30-100 ℃, and the precipitation is carried out until the pH value of the mixed solution is 5.5-7.5; (3) and precipitating the mixed solution until the pH value is 5.5-7.5, washing and filtering to obtain the high-aluminum-content rare earth precipitate, so that the aluminum-content rare earth liquid is precipitated by using the method, the aluminum-removal step is not needed, the precipitation process is smooth, and the precipitate is loose in particles and easy to wash and filter. The removal rate of aluminum can reach 80 percent after the obtained precipitate is completely precipitated; the removal rate of aluminum of the precipitate obtained by incomplete precipitation can reach more than 99 percent. After the precipitate is burned, sulfosalicylic acid has no residue, and no new impurity is introduced.
Description
Technical Field
The invention relates to the field of rare earth hydrometallurgy and inorganic chemistry, in particular to a precipitation method of an aluminum-containing rare earth feed liquid.
Background
The precipitation process of rare earth carbonate is influenced by many factors, such as temperature, concentration, impurity content, etc. Among the impurities, iron and aluminum have a particularly remarkable influence on the precipitation of rare earth carbonate. The whole process of carbonate precipitation is mainly carried out under the condition of pH 4-6, but the pH value of iron ions which start to hydrolyze is 1.5, and the pH value of iron ions which are completely hydrolyzed is 4.1; the pH value of the beginning hydrolysis of aluminum ions is 3.3, the pH value of the complete hydrolysis is 5.2, namely, the hydrolysis of iron and aluminum already occurs when the carbonate precipitation is just started, iron hydroxide and aluminum hydroxide generated by the hydrolysis are colloidal substances and have fine particles, and the colloidal substances exist as seed crystals in the precipitation process, so that the subsequent generated carbonate particles are fine, and even the precipitation cannot be carried out. Therefore, impurities in the feed liquid are removed before carbonate precipitation in the industry. The existing methods for separating rare earth from aluminum mainly comprise the following steps:
1. adjusting pH value to make iron and aluminum hydrolyze preferentially and separate rare earth feed liquid. Such as: a green separation method of impurity aluminum element in rare earth concentrate (CN 202010241167.2); a method for removing regular impurities in waste rare earth polishing powder (CN 109536037A); method for removing impurity aluminum in rare earth fluocarbonate ore leaching process (CN 201410511341.5)
2. Extraction and separation: the separation is carried out by utilizing the extraction separation of iron and aluminum and rare earth. Such as "method for extracting and recovering rare earth from low-content rare earth solution by using primary amine extractant" (CN 201610820708.0); a method for continuously extracting aluminum from rare earth feed liquid (CN 201410191827.5); method for removing aluminum from rare earth feed liquid (CN 201010547720.1)
3. Oxalate precipitates, and oxalic acid and iron and aluminum mainly form a complex and exist in a liquid phase, so that the aim of separating the oxalate from solid-phase rare earth oxalate is fulfilled. Such as: a method for recovering rare earth from a rare earth-containing aluminum-silicon material (publication No. CN 101705380A); method for recovering rare earth from waste aluminate green rare earth fluorescent powder (publication No. CN 201410305236.6)
4. Carrying out precipitation separation by utilizing the difference of complexing abilities of a complexing agent to aluminum and rare earth: such as "a method for separating rare earth and aluminum by complexation" (publication No. CN 1089502068); a method for removing aluminum by complexing and precipitating from a rare earth solution (publication No. CN 105624440A); method for removing aluminum from rare earth feed liquid by complexing precipitation (publication No. CN 1086423018)
Among the above methods, the method 1 and the method 4 have various steps and need filtration and separation, and some methods have difficulty in filtration due to fine solid phase particles; the method 2 has large occupied area, long time and high cost; in the method 3, the price of oxalic acid is higher; the method provided by the invention can effectively improve the precipitation environment of the rare earth carbonate without removing aluminum in advance and adding any step, and has the advantages of less reagent dosage and extremely low cost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a precipitation method of high-aluminum rare earth feed liquid, which has simple production process, simple and convenient operation and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a precipitation method of an aluminum-containing rare earth feed liquid comprises the following steps: (1) taking the aluminum-containing rare earth feed liquid flowing out of the extraction tank, adding water into the aluminum-containing rare earth feed liquid for dilution, diluting the aluminum-containing rare earth feed liquid to 80g/L, adding an aluminum complexing agent, and uniformly stirring to obtain a mixed solution; (2) adding a precipitator into the mixed solution for precipitation, wherein the precipitation temperature is 30-100 ℃, and the precipitation is carried out until the pH = 5.5-7.5 of the mixed solution; (3) and precipitating the mixed solution until the pH = 5.5-7.5, washing and filtering to obtain the high-aluminum-content rare earth precipitate.
Further, the aluminum-containing rare earth material liquid in the step 1 comprises one or more combinations of a praseodymium neodymium chloride material liquid, a cerium rare earth chloride material liquid and a rare earth nitrate material liquid, and the concentrations of the praseodymium neodymium chloride material liquid, the cerium rare earth chloride material liquid and the rare earth nitrate material liquid are all 10-200 g/L.
Further, the complexing agent of the aluminum in the step 1 is sulfosalicylic acid, and the molar ratio of the sulfosalicylic acid to the aluminum in the aluminum-containing rare earth feed liquid is 3-1: 1.
Further, the precipitant in step 2 includes ammonium bicarbonate, sodium bicarbonate, ammonium carbonate, and sodium carbonate.
Further, the precipitation in the step 2 is performed according to a precipitation process of rare earth carbonate.
Compared with the prior art, the invention has the following beneficial effects:
the method for precipitating the aluminum-containing rare earth feed liquid does not need the step of removing aluminum, has smooth precipitation process, loose precipitate particles and is easy to wash and filter. The removal rate of aluminum can reach 80 percent after the obtained precipitate is completely precipitated; the removal rate of aluminum of the precipitate obtained by incomplete precipitation can reach more than 99 percent. After the precipitate is burned, sulfosalicylic acid has no residue, and no new impurity is introduced.
Detailed Description
To make the technical problems, technical solutions and advantages to be solved by the present invention clearer. In the following description, characteristic details such as specific configurations and components are provided only to help the embodiments of the present invention be fully understood. Thus, it will be apparent to those skilled in the art that various changes and modifications may be made to the embodiments described herein without departing from the scope and spirit of the invention. In addition, descriptions of well-known functions and constructions are omitted for clarity and conciseness.
It should be appreciated that reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
In various embodiments of the present invention, it should be understood that the sequence numbers of the following processes do not mean the execution sequence, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present invention.
It should be understood that the term "and/or" herein is merely one type of association relationship that describes an associated object, meaning that three relationships may exist, e.g., a and/or B may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
In the embodiments provided herein, it should be understood that "B corresponding to a" means that B is associated with a from which B can be determined. It should also be understood that determining B from a does not mean determining B from a alone, but may be determined from a and/or other information.
The invention provides a precipitation method of an aluminum-containing rare earth feed liquid.
Example 1
2000ml of praseodymium neodymium chloride feed liquid (PN) taken from the effluent of the extraction tank2O3 187/L，Al2O3 0.4g/L，Fe2O30.1 g/L), adding water into the praseodymium neodymium chloride feed liquid for dilution, so that the praseodymium neodymium chloride feed liquid is diluted to 80g/L, and adding 4g of sulfosalicylic acid, wherein the molar ratio of the sulfosalicylic acid to aluminum in the praseodymium neodymium chloride feed liquid is 1: 1; precipitating with ammonium bicarbonate at 60 deg.C. Precipitating until the pH is =6.4, then washing and filtering to obtain precipitate praseodymium neodymium carbonate, wherein the measured total amount of the precipitate praseodymium neodymium carbonate is 47.3 percent, and Cl is obtained- 0.017%,Al2O3% is 0.0335%.
Example 2
2000ml of cerium chloride solution (CeO) taken from the effluent of the extraction tank2 217/L，Al2 O3 0.056g/L，Fe2O30.01 g/L), adding water into the cerium chloride feed liquid for dilution to ensure that the cerium chloride feed liquid is diluted to 80g/L, and adding 0.56g of sulfosalicylic acid, wherein the molar ratio of the sulfosalicylic acid to aluminum in the cerium chloride feed liquid is 1: 1; precipitating with ammonium bicarbonate at 55 deg.C. Precipitating to pH =5.6, washing, and filtering to obtain precipitate cerium carbonate, wherein the total amount of the precipitate cerium carbonate is 51.3%, and Cl is detected- 0.011%,Al2O3% is 0.0025%.
Example 3
2000ml of praseodymium neodymium chloride feed liquid (PN) taken from the effluent of the extraction tank2O3 187/L，Al2O3 0.4g/L，Fe2O30.1 g/L), adding water into the praseodymium neodymium chloride feed liquid for dilution, so that the praseodymium neodymium chloride feed liquid is diluted to 80g/L, and adding 12g of sulfosalicylic acid, wherein the molar ratio of the sulfosalicylic acid to aluminum in the praseodymium neodymium chloride feed liquid is 3: 1; precipitating with ammonium bicarbonate at 60 deg.C. Precipitating until the pH is =7.1, then washing and filtering to obtain a precipitate praseodymium neodymium carbonate, wherein the total praseodymium carbonate content is measured to be 50.3%, Cl- 0.018%,Al2O3% is 0.038%. After firing, the total content of praseodymium neodymium oxide measured is 99.3%, Al2O3% is 0.075% and bulk specific gravity is 1.36 g/ml.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the technical solutions of the present invention have been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that the technical solutions described in the foregoing embodiments can be modified or some technical features can be replaced equally; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. A precipitation method of an aluminum-containing rare earth feed liquid is characterized by comprising the following steps: the method comprises the following steps:
(1) taking the aluminum-containing rare earth feed liquid flowing out of the extraction tank, adding water into the aluminum-containing rare earth feed liquid for dilution, diluting the aluminum-containing rare earth feed liquid to 80g/L, adding an aluminum complexing agent, and uniformly stirring to obtain a mixed solution;
(2) adding a precipitator into the mixed solution for precipitation, wherein the precipitation temperature is 30-100 ℃, and the precipitation is carried out until the pH value of the mixed solution is 5.5-7.5;
(3) and precipitating the mixed solution until the pH value is 5.5-7.5, washing and filtering to obtain the high-aluminum-content rare earth precipitate.
2. The method for precipitating the aluminum-containing rare earth feed liquid according to claim 1, wherein the method comprises the following steps: the aluminum-containing rare earth material liquid in the step 1 comprises one or more combinations of a praseodymium neodymium chloride material liquid, a cerium chloride rare earth material liquid and a rare earth nitrate material liquid, and the concentrations of the praseodymium neodymium chloride material liquid, the cerium chloride rare earth material liquid and the rare earth nitrate material liquid are all 10-200 g/L.
3. The method for precipitating the aluminum-containing rare earth feed liquid according to claim 1, wherein the method comprises the following steps: the complexing agent of the aluminum in the step 1 is sulfosalicylic acid, and the molar ratio of the sulfosalicylic acid to the aluminum in the aluminum-containing rare earth feed liquid is 3-1: 1.
4. The method for precipitating the aluminum-containing rare earth feed liquid according to claim 1, wherein the method comprises the following steps: and the precipitant in the step 2 comprises ammonium bicarbonate, sodium bicarbonate, ammonium carbonate and sodium carbonate.
5. The method for precipitating the aluminum-containing rare earth feed liquid according to claim 1, wherein the method comprises the following steps: the precipitation in the step 2 is performed according to a precipitation process of rare earth carbonate.
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2021
- 2021-06-24 CN CN202110705546.7A patent/CN113604686A/en active Pending
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