CN111926181A - Method for stepwise recovering valuable components in rare earth concentrate - Google Patents
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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Abstract
The invention relates to a method for recovering valuable components in rare earth concentrate step by step, which comprises the following steps: (1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution; (2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P; (3) and (3) performing acid leaching on the leaching residue obtained in the step (2) to obtain a solution containing cerium and thorium. The final recovery rate of Th is more than 95%, the recovery rates of F and P are more than 90%, the recovery rate of rare earth is more than 95%, the process is stable, no waste gas and radioactive waste residues exist, the recovery process of non-cerium rare earth accounting for 75% of economic value is short, and economic benefit is high.
Description
Technical Field
The invention relates to the field of rare earth recovery, in particular to a method for recovering valuable components in rare earth concentrate step by step.
Background
Rare earth is called industrial gold, and can be combined with other materials to form novel materials with various performances and varieties due to excellent physical properties such as photoelectromagnetism and the like. Therefore, rare earth has irreplaceable effects in the fields of metallurgical industry, petrochemical industry, glass ceramics, agriculture, new materials and the like.
The most representative mineral of Chinese rare earth resource-Baobaiyibobo rare earth ore is mainly composed of two minerals of bastnaesite and monazite, and the rare earth concentrate formed by mineral separation also mainly consists of the two minerals. At present, the main smelting production process of Baotou rare earth concentrate is a concentrated sulfuric acid high-temperature rotary kiln roasting process. Although there are many important scientific achievements in the hydrometallurgy industry, which is crucial to the development of the rare earth industry in China, with the development of science and technology and the increase of environmental awareness and strength, the process exposes a lot of outstanding problems:
1. the problem of three wastes is difficult to solve. 2. During the high-temperature roasting process of concentrated sulfuric acid, tail gas of F and S is generated, and the production cost is increased by flue gas absorption. 3. The F and P in the minerals are not recovered as valuable chemicals. 4. The cerium which accounts for half of the total rare earth has low value, and the total rare earth extraction separation process has long flow and low economic benefit. 5. After the concentrated sulfuric acid decomposes minerals, the rare earth sulfate is prepared by water immersion, and before the rare earth sulfate enters an extraction process section, the rare earth sulfate needs to be further transformed into rare earth chloride, and ammonia nitrogen wastewater is additionally generated in the transformation process.
In order to meet the rapid development and continuously enlarged production scale of the rare earth industry, improvement and perfection of rare earth smelting processes, including aspects of environmental protection, consumption reduction, comprehensive resource utilization and the like, even innovation of the processes is urgently needed. In recent years, through the efforts of science and technology workers, a sodium hydroxide decomposition process, a concentrated sulfuric acid low-temperature roasting decomposition process, a sodium carbonate roasting decomposition process and the like are researched and developed. However, these processes are still only in the laboratory due to various problems.
CN102277483A proposes a new method for preparing rare earth chloride from Bayan Obo rare earth concentrate, although the method also proposes that the rare earth concentrate is roasted by air firstly, then the rare earth chloride is prepared by hydrochloric acid leaching, and finally alkali decomposition is adopted for acid leaching slag. However, in the process of hydrochloric acid leaching, all rare earth is converted into rare earth chloride, and the economic benefit of extraction separation is not considered, because cerium (which accounts for about half of the total rare earth) with low value is also completely converted into rare earth chloride, the cost of subsequent rare earth extraction separation is high, and the economic benefit is low.
CN103397213A proposes to treat Baotou rare earth concentrate with mixed alkali (sodium hydroxide and sodium carbonate) first, but in order to reduce the consumption of alkali and solve the agglomeration phenomenon during roasting, they first remove iron and calcium by chemical method. The mixed alkali provided by the patent decomposes the rare earth concentrate, belongs to typical solid-solid reaction, has low efficiency and has higher requirement on the taste of the concentrate.
Therefore, research and development of a clean production process for smelting and separating rare earth ore, improvement of resource utilization rate, reduction of unit consumption, solving of the problem of three-waste pollution, improvement of economic benefits of enterprise production, and guarantee of stable operation of a smelting process are problems to be solved urgently aiming at smelting of Baotou rare earth ore at present.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a method for recovering valuable components in rare earth concentrate step by step, which realizes the distribution and separation of valuable elements in the rare earth concentrate by a coupling process of fluidized roasting-alkali liquor treatment, can separate F and P independently, has a Th recovery rate of more than 95%, F and P recovery rates of more than 90%, a rare earth recovery rate of more than 95%, a stable process, no waste gas and radioactive waste residues, a short non-cerium rare earth recovery flow accounting for 75% of economic value and high economic benefit.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for recovering valuable components in rare earth concentrate step by step, which comprises the following steps:
(1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution;
(2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P;
(3) and (3) performing acid leaching on the leaching residue obtained in the step (2) to obtain a solution containing cerium and thorium.
The invention adopts the fluidization state roasting technology to process Baotou rare earth concentrate. In the roasting process, bastnaesite in Baotou rare earth concentrate is decomposed, Ce3+Is simultaneously oxidized to Ce4+Being cerium and trivalentThe separation of rare earth creates conditions. And then, optimally leaching with hydrochloric acid, preferentially leaching non-cerium trivalent rare earth, and performing filter pressing separation to obtain a cerium-less rare earth solution and thorium-containing cerium-rich ore. And decomposing monazite in the solution by using a sub-molten salt technology. After mineral decomposition is completed, adding hot water for aging, washing and filtering, and allowing F and P and excessive alkali to enter water washing liquid for extracting and separating F and P, and finally recovering Th>95% recovery of F and P>90 percent, the recovery rate of the rare earth is more than 95 percent, the process is stable, no waste gas and radioactive waste residue exist, the recovery flow of the non-cerium rare earth accounting for 75 percent of the economic value is short, and the economic benefit is high.
The aging in the invention is to add water to the mixture treated by the alkali liquor for treatment.
The solution containing cerium and thorium also contains a small amount of trivalent rare earth.
In a preferred embodiment of the present invention, the content of the bastnaesite and the monazite in the rare earth concentrate of the step (1) is 45 to 65% by mass, for example, 45%, 50%, 55%, 60%, or 65% by mass, but not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
As a preferred embodiment of the present invention, the fluidized roasting temperature in the step (1) is 400-600 ℃, for example, 400 ℃, 450 ℃, 500 ℃, 550 ℃ or 600 ℃, but not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the fluidized roasting time is 1-2h, for example, 1h, 1.2h, 1.4h, 1.6h, 1.8h or 2h, etc., but not limited to the recited values, and other values not recited in the range are also applicable.
In the fluidized roasting process, the particles continuously move under the action of hot air flow, and the particles are decomposed in the movement process. As a preferable technical scheme of the invention, the roasted rare earth concentrate is subjected to slurrying before the hydrochloric acid in the step (1) is dissolved preferentially.
Preferably, the solid-to-liquid ratio g/mL in the slurry is 1 (2-3), and may be, for example, 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, or 1:3, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
As a preferred embodiment of the present invention, the flow rate of the hydrochloric acid solution in the hydrochloric acid optimum solution in the step (1) is 20 to 30L/min, for example, 20L/min, 22L/min, 24L/min, 26L/min, 28L/min, or 30L/min, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the concentration of the hydrochloric acid solution in the hydrochloric acid preferential solution in the step (1) is 20-35%, for example, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34% or 35%, etc., but is not limited to the recited values, and other values not recited in the range are also applicable.
As a preferred embodiment of the present invention, the temperature of the hydrochloric acid solution in the step (1) is 50 to 80 ℃ and may be, for example, 50 ℃, 60 ℃, 70 ℃ or 80 ℃, but not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the preferential dissolution time of the hydrochloric acid in the step (1) is 2 to 5 hours, such as 2 hours, 3 hours, 4 hours or 5 hours, but not limited to the enumerated values, and other unrecited values in the range are also applicable.
Preferably, the end point of the hydrochloric acid dissolution optimization in step (1) is a solution pH of 1-2, such as 1, 1.2, 1.4, 1.6, 1.8 or 2, but not limited to the recited values, and other values not recited in this range are also applicable.
The optimal dissolution of hydrochloric acid is to control the dosage of acid, so that trivalent rare earth which is better dissolved is dissolved in the solution in the form of chloride, and tetravalent cerium which is difficult to dissolve is not dissolved out and is left in slag. If the optimum solution is not adopted, but excessive hydrochloric acid is adopted for dissolving, the quadrivalent cerium can be partially dissolved due to the reducibility of the hydrochloric acid and enters the solution together with the trivalent rare earth, so that the pressure is brought to the subsequent extraction and separation, the reagent loss is large, the flow is long, and the economic benefit is low.
As a preferred embodiment of the present invention, the concentration of the alkali solution used in the alkali solution treatment in step (2) is 40 to 70% by mass, for example, 40%, 50%, 60% or 70% by mass, but not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the temperature of the alkali treatment in step (2) is 140-180 ℃, such as 140 ℃, 150 ℃, 160 ℃, 170 ℃ or 180 ℃, but not limited to the enumerated values, and other unrecited values in the range are also applicable.
Preferably, the time of the alkaline treatment in step (2) is 3-5h, such as 3h, 3.5h, 4h, 4.5h or 5h, but not limited to the recited values, and other values not recited in the range are also applicable.
The alkali solution in the alkali solution treatment in the present invention may be a sodium hydroxide solution or the like.
As a preferred embodiment of the present invention, the temperature of aging in the step (2) is 95 to 105 ℃, for example, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃, 100 ℃, 101 ℃, 102 ℃, 103 ℃, 104 ℃ or 105 ℃, etc., but not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the aging time in step (2) is 1 to 2 hours, and may be, for example, 1 hour, 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2 hours, etc., but is not limited to the recited values, and other values not recited in the range are also applicable.
When the solid-liquid separation is carried out after the aging in the invention, the filter cake is washed by water in the filter press until the adsorbed soluble substances are basically washed out, and the contents of F and P are lower than 0.3 percent.
In a preferred embodiment of the present invention, the acid solution used in the acid leaching in step (3) may have a concentration of 10 to 50% by mass, for example, 10%, 20%, 30%, 40%, or 50%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable. The acid solution is sulfuric acid solution, etc.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution; the temperature of the fluidized roasting is 400-600 ℃; the fluidized roasting time is 1-2 h;
(2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P; the mass percentage concentration of the alkali liquor used in the alkali liquor treatment is 40-70%; the temperature of the alkali liquor treatment is 140-180 ℃; the time for treating the alkali liquor is 3-5 h;
(3) and (3) performing acid leaching on the leaching residue obtained in the step (2) to obtain a solution containing cerium and thorium.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) the invention realizes the fractional recovery of the valuable components, F, P and Th in the Baotou rare earth concentrate by utilizing the coupling effect between the fluidized roasting and the alkali liquor treatment.
(2) According to the invention, the final recovery rate of Th is more than 95%, the recovery rates of F and P are more than 90%, the recovery rate of rare earth is more than 95%, the process is stable, no waste gas and radioactive waste residues exist, the recovery process of non-cerium rare earth accounting for 75% of economic value is short, and the economic benefit is high.
Drawings
Fig. 1 is a schematic diagram of a method for stepwise recovering valuable components from rare earth concentrates, which is provided in embodiment 1 of the invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
In the embodiment, the rare earth concentrate is Baotou rare earth concentrate, the composition of the Baotou rare earth concentrate is that the proportion of the bastnaesite to the monazite is 3:2, and the grade of the rare earth concentrate is 50 percent
The rare earth concentrate is treated by the following method, as shown in figure 1:
(1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution; the temperature of the fluidized roasting is 500 ℃; the fluidized roasting time is 1.5 h; before the hydrochloric acid is dissolved preferentially, the roasted rare earth concentrate is subjected to slurrying; the solid-liquid ratio g/mL in the slurrying is 1: 2.5; the flow rate of the hydrochloric acid solution in the preferential solution of the hydrochloric acid is 25L/min; the concentration of the hydrochloric acid solution in the preferential solution of the hydrochloric acid is 25 percent; the temperature of preferential dissolution of the hydrochloric acid is 66 ℃; the preferential dissolution time of the hydrochloric acid is 3.2 h; the final point of the preferential dissolution of the hydrochloric acid is that the pH value of the solution is 1.5;
(2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P; the mass percentage concentration of the alkali liquor (sodium hydroxide solution) used in the alkali liquor treatment is 56 percent; the temperature of the alkali liquor treatment is 160 ℃; the time for treating the alkali liquor is 4 hours; the aging temperature is 100 ℃; the aging time is 1.5 h;
(3) and (3) carrying out acid leaching on the leaching residue obtained in the step (2) by adopting 33% sulfuric acid to obtain a solution containing cerium, thorium and trivalent rare earth.
The recovery rate of cerium is 96.5%, the recovery rate of thorium is 95.5%, the recovery rates of F and P are 91%, and the recovery rate of trivalent rare earth is 98%.
Example 2
In the embodiment, the rare earth concentrate is Baotou rare earth concentrate, the proportion of the bastnaesite to the monazite is 3:1, and the grade of the rare earth concentrate is 55%;
the rare earth concentrate is treated by adopting the following method:
(1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution; the temperature of the fluidized roasting is 400 ℃; the fluidized roasting time is 2 hours; before the hydrochloric acid is dissolved preferentially, the roasted rare earth concentrate is subjected to slurrying; the solid-liquid ratio g/mL in the slurrying is 1: 3; the flow rate of the hydrochloric acid solution in the preferential solution of the hydrochloric acid is 20L/min; the concentration of the hydrochloric acid solution in the hydrochloric acid optimum solution is 35 percent; the temperature of preferential dissolution of the hydrochloric acid is 80 ℃; the preferential dissolution time of the hydrochloric acid is 2 hours; the end point of the preferential dissolution of the hydrochloric acid is that the pH value of the solution is 2;
(2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P; the mass percentage concentration of the alkali liquor (sodium hydroxide solution) used in the alkali liquor treatment is 70 percent; the temperature of the alkali liquor treatment is 180 ℃; the time for treating the alkali liquor is 3 hours; the temperature of the aging is 95 ℃; the aging time is 1 h;
(3) and (3) carrying out acid leaching on the leaching residue obtained in the step (2) by adopting 12% sulfuric acid to obtain a solution containing cerium, thorium and trivalent rare earth.
The recovery rate of cerium is 95.9%, the recovery rate of thorium is 96.5%, the recovery rates of F and P are 92%, and the recovery rate of trivalent rare earth is 98.5%.
Example 3
In the embodiment, the rare earth concentrate is Baotou rare earth concentrate, the proportion of the bastnaesite to the monazite is 5:1, and the grade of the rare earth concentrate is 60%; the rare earth concentrate is treated by adopting the following method:
(1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution; the temperature of the fluidized roasting is 600 ℃; the fluidized roasting time is 1 h; before the hydrochloric acid is dissolved preferentially, the roasted rare earth concentrate is subjected to slurrying; the solid-liquid ratio g/mL in the slurrying is 1: 2; the flow rate of the hydrochloric acid solution in the preferential solution of the hydrochloric acid is 30L/min; the concentration of the hydrochloric acid solution in the hydrochloric acid optimum solution is 20%; the temperature of preferential dissolution of the hydrochloric acid is 50 ℃; the preferential dissolution time of the hydrochloric acid is 5 hours; the end point of the preferential dissolution of the hydrochloric acid is that the pH value of the solution is 1;
(2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P; the mass percentage concentration of the alkali liquor (sodium hydroxide solution) used in the alkali liquor treatment is 40 percent; the temperature of the alkali liquor treatment is 140 ℃; the time for treating the alkali liquor is 5 hours; the temperature of the aging is 105 ℃; the aging time is 2 h;
(3) and (3) performing acid leaching on the leaching residue obtained in the step (2) by adopting 50% sulfuric acid to obtain a solution containing cerium, thorium and trivalent rare earth.
The recovery rate of cerium is 97%, the recovery rate of thorium is 96.6%, the recovery rates of F and P are 93%, and the recovery rate of trivalent rare earth is 99%.
Comparative example 1
The only difference from example 1 is that the fluidized roasting was replaced by conventional roasting, the recovery of cerium was 87%, the recovery of thorium was 86.6%, the recovery of F and P was 85%, and the recovery of trivalent rare earths was 79%.
Comparative example 2
The only difference from example 1 is that the hydrochloric acid optimum dissolution was replaced by sulfuric acid dissolution under the same conditions, the recovery of cerium was 85%, the recovery of thorium was 87%, the recovery of F and P was 80%, and the recovery of trivalent rare earth was 72%.
Comparative example 3
The only difference from example 1 is that without aging, the recovery of cerium was 88%, the recovery of thorium was 88%, the recovery of F and P was 83%, and the recovery of trivalent rare earths was 82%.
According to the results of the above examples and comparative examples, the present invention adopts the fluidized state roasting technology to treat Baotou rare earth concentrates. In the roasting process, bastnaesite in Baotou rare earth concentrate is decomposed, Ce3+Is simultaneously oxidized to Ce4+And conditions are created for separation of cerium and trivalent rare earth. And then, optimally leaching with hydrochloric acid, preferentially leaching non-cerium trivalent rare earth, and performing filter pressing separation to obtain a cerium-less rare earth solution and thorium-containing cerium-rich ore. And decomposing monazite in the solution by using a sub-molten salt technology. After mineral decomposition is completed, adding hot water for aging, washing and filtering, and allowing F and P and excessive alkali to enter water washing liquid for extracting and separating F and P, and finally recovering Th>95% recovery of F and P>90 percent, the recovery rate of the rare earth is more than 95 percent, the process is stable, no waste gas and radioactive waste residue exist, the recovery flow of the non-cerium rare earth accounting for 75 percent of the economic value is short, and the economic benefit is high.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A method for recovering valuable components in rare earth concentrates step by step is characterized by comprising the following steps:
(1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution;
(2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P;
(3) and (3) performing acid leaching on the leaching residue obtained in the step (2) to obtain a solution containing cerium and thorium.
2. The recovery method according to claim 1, wherein the bastnaesite and monazite are contained in the rare earth concentrate of the step (1) in a mass percentage of 45 to 65%.
3. The method as claimed in claim 1 or 2, wherein the temperature of the fluidized roasting in the step (1) is 400-600 ℃;
preferably, the time of fluidized roasting is 1-2 h.
4. The method of any one of claims 1 to 3, wherein the calcined rare earth concentrate is slurried before the hydrochloric acid is preferentially dissolved in step (1);
preferably, the solid-to-liquid ratio g/mL in the slurrying is 1 (2-3).
5. The method according to any one of claims 1 to 4, wherein the flow rate of the hydrochloric acid solution in the preferential dissolution of hydrochloric acid in the step (1) is 20 to 30L/min;
preferably, the concentration of the hydrochloric acid solution in the hydrochloric acid preferential solution in the step (1) is 20-35%.
6. The method according to any one of claims 1 to 5, wherein the temperature of preferential dissolution of hydrochloric acid in step (1) is 50 to 80 ℃;
preferably, the preferential dissolution time of the hydrochloric acid in the step (1) is 2-5 h;
preferably, the final point of the hydrochloric acid preferential dissolution in the step (1) is that the pH value of the solution is 1-2.
7. The method of any one of claims 1 to 6, wherein the concentration of the lye used in the lye treatment of step (2) is from 40 to 70% by mass;
preferably, the temperature of the alkali treatment in the step (2) is 140-180 ℃;
preferably, the time of the alkali liquor treatment in the step (2) is 3-5 h.
8. The method according to any one of claims 1 to 7, wherein the temperature of aging in step (2) is 95 to 105 ℃;
preferably, the aging time of step (2) is 1-2 h.
9. The process according to any one of claims 1 to 8, wherein the acid liquor used in the acid leaching in step (3) has a concentration of 10 to 50% by mass.
10. A method according to any one of claims 1-9, characterized in that the method comprises the steps of:
(1) sequentially carrying out fluidized roasting and hydrochloric acid preferential dissolution on the rare earth concentrate, and then carrying out solid-liquid separation to obtain thorium-containing cerium-rich ore and trivalent rare earth solution; the temperature of the fluidized roasting is 400-600 ℃; the fluidized roasting time is 1-2 h;
(2) sequentially carrying out alkali liquor treatment and aging on the thorium-containing cerium-rich ore obtained in the step (1), and then carrying out solid-liquid separation to obtain washing slag and a solution containing F and P; the mass percentage concentration of the alkali liquor used in the alkali liquor treatment is 40-70%; the temperature of the alkali liquor treatment is 140-180 ℃; the time for treating the alkali liquor is 3-5 h;
(3) and (3) performing acid leaching on the leaching residue obtained in the step (2) to obtain a solution containing cerium and thorium.
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| CN202010837734.0A CN111926181A (en) | 2020-08-19 | 2020-08-19 | Method for stepwise recovering valuable components in rare earth concentrate |
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