CN114752788A - Roasting method of rare earth ore concentrate added with active agent - Google Patents
Roasting method of rare earth ore concentrate added with active agent Download PDFInfo
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- 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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Abstract
The invention relates to a roasting method of rare earth ore concentrate added with an active agent, which comprises the following steps of A, adding the active agent into the rare earth ore concentrate, fully mixing, roasting at the temperature of 600-950 ℃, wherein the roasting time is 0.5-2.5 hours; the adding amount of the active agent is 5-30% of the mass of the rare earth concentrate; the active agent is active carbon, and the rare earth concentrate is rare earth mixed ore. The invention has the beneficial effects that: can effectively improve the acid dissolution leaching rate of the rare earth, reduce the environmental pollution and reduce the production cost of enterprises, and has important social and economic meanings.
Description
Technical Field
The invention relates to the field of rare earth, in particular to a roasting method of rare earth ore concentrate added with an active agent.
Background
Rare earth ores are classified into bastnaesite and ionic ores, the bastnaesite has rare earth phosphate, monazite containing no rare earth fluoride, tetrachorite containing no rare earth phosphate, and rare earth mixed ores containing both rare earth fluoride and rare earth phosphate (e.g., baotite and american ores).
The common smelting process of several rare earth ores comprises the following steps:
monazite ore: alkali conversion production method. The monazite concentrate is made into powder, then the powder is converted into phosphorus by sodium hydroxide, and the phosphorus is dissolved by hydrochloric acid to obtain a rare earth chloride solution.
Sichuan mine: oxidizing roasting-alkali conversion method. Adding the rare earth concentrate into a rotary kiln, carrying out oxidizing roasting at the temperature of about 750 ℃, dissolving the roasted ore with hydrochloric acid to obtain a chlorinated rare earth solution, wherein the hydrochloric acid can leach about 60% of rare earth in the rare earth ore. And (3) alkali-converting acid-soluble residues dissolved by hydrochloric acid by using sodium hydroxide to remove fluorine, and dissolving rare earth in the leached residues by using the hydrochloric acid. This process produces rare earth slag, which is high in rare earth content and causes rare earth loss.
Baotite is divided into two production processes: one is the sulfuric acid roasting process. And mixing the rare earth concentrate with concentrated sulfuric acid, adding into a rotary kiln, roasting at the temperature of about 850 ℃, leaching roasted ore with water to obtain rare earth sulfate, and extracting and transforming the rare earth sulfate by p204 to obtain a rare earth chloride solution. And secondly, an oxidizing roasting-alkali conversion method (adopting a Sichuan ore production process), wherein rare earth concentrate is subjected to calcium washing by using dilute hydrochloric acid, the washed calcium ore enters a rotary kiln, the calcium is subjected to oxidizing roasting at the temperature of about 800 ℃, hydrochloric acid for roasting ore is dissolved to obtain a rare earth chloride solution, about 32% of rare earth in the rare earth ore can be leached by hydrochloric acid dissolution, acid-soluble slag after hydrochloric acid dissolution is subjected to alkali conversion by using sodium hydroxide to remove fluorine and phosphorus, and the rare earth in the leached slag is dissolved by using the hydrochloric acid.
Through serious research and analysis on the smelting production process of the rare earth ore, the lowest production cost of oxidizing roasting and the lowest environmental protection investment are found. The more rare earth is obtained by leaching the rare earth ore with hydrochloric acid after oxidizing roasting, the lower the production cost of the rare earth. Based on this consideration, we have conducted earnest research and experiments on the process of oxidizing and roasting bastnasite.
Therefore, in order to improve the yield of the rare earth obtained by oxidizing roasting, the scheme provides the roasting method of the rare earth ore concentrate added with the active agent, and the method can improve the yield of the rare earth, reduce the environmental pollution and reduce the production cost of enterprises, and has important social and economic meanings.
Disclosure of Invention
The invention aims to overcome the defects and provide the roasting method of the rare earth ore concentrate added with the activating agent, and the roasting method can effectively improve the rare earth yield, reduce the environmental pollution and reduce the production cost of enterprises, and has important social and economic meanings. The purpose of the invention is realized by the following technical scheme:
a roasting method of rare earth ore concentrate added with an active agent comprises the following steps:
step A, adding an active agent into rare earth concentrate, fully mixing and roasting; preferably, the roasting temperature is 600-950 ℃, and the roasting time is 0.5-2.5 hours;
the adding amount of the active agent is 5-30% of the mass of the rare earth concentrate;
the active agent is active carbon, and the rare earth concentrate is rare earth mixed ore.
Further, the rare earth mixed ore is Baotou rare earth concentrate or American ore rare earth concentrate.
As a preferred mode, the roasting method of the rare earth ore concentrate added with the active agent comprises the following steps:
step A, adding activated carbon into rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2 hours;
the adding amount of the active agent is 15% of the mass of the rare earth concentrate;
the rare earth concentrate is Baotou rare earth concentrate.
Further, the roasting method of the rare earth ore concentrate added with the active agent also comprises a step B;
and step B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag.
Preferably, the particle size of the activated carbon is 4-200 meshes.
Furthermore, the roasting method of the rare earth ore concentrate added with the active agent further comprises a step C;
c, extracting the residual rare earth in the acid leaching residue by using the acid leaching residue obtained in the step B through a sulfuric acid roasting method process;
and C, specifically, mixing concentrated sulfuric acid with the acid leaching residue obtained in the step B, adding the acid leaching residue into a rotary kiln, roasting at the temperature of about 850 ℃ to obtain roasted ore, leaching the roasted ore with water to obtain rare earth sulfate, and extracting and transforming the rare earth sulfate by using p204 to obtain a rare earth chloride solution.
Furthermore, the roasting method of the rare earth ore concentrate added with the active agent also comprises a step C';
c', removing fluorine and phosphorus from the acid leaching residue obtained in the step B by a sodium hydroxide alkali conversion method, dissolving by hydrochloric acid, and leaching rare earth;
and C, adding sodium hydroxide into the acid leaching residue obtained in the step B, performing alkali conversion to obtain an alkali-converted ore, filtering, washing with water, adding hydrochloric acid into the washed alkali-converted ore to dissolve, and leaching rare earth to obtain a rare earth chloride solution and acid leaching residue.
Preferably, the roasting method of the rare earth ore concentrate added with the active agent further comprises the steps of A0 before the step A;
and A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate. The calcium content of baotite is high, which affects the extraction and separation of subsequent rare earth, so that the calcium is washed from high-grade rare earth ore before roasting, so as to reduce the treatment cost of the subsequent extraction process; the final calcium content required by calcium washing can be determined according to the requirement of extraction process on calcium during production.
Further, the step B specifically comprises the steps of: adding hydrochloric acid with the concentration of 30% into the roasted rare earth concentrate, heating to 95 ℃, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain rare earth chloride solution and acid leaching slag.
Compared with the prior art, the invention has the beneficial effects that:
32% of rare earth can be leached out by hydrochloric acid after Baotou ore raw ore is oxidized and roasted, and the leached part of rare earth can be lanthanum-cerium-carbon rare earth which is not combined with phosphorus and fluorine; when activated carbon is added for roasting, the activity of the rare earth element is improved under the action of the activator, so that more rare earth is dissolved by hydrochloric acid, and the leaching rate of the rare earth is improved to 52%; further, the yield of the rare earth of the oxidizing roasting is further improved, and the characteristics of lowest production cost and lowest environmental protection investment of the oxidizing roasting are combined, so that the scheme further reduces the environmental pollution and the production cost of enterprises, and has important social significance and economic significance.
Detailed Description
Example 1
A preferred embodiment of a roasting method of rare earth ore concentrate to which an active agent is added, comprising the steps of:
step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2 hours; the adding amount of the active agent is 15 percent of the mass of the rare earth concentrate;
wherein the active agent is activated carbon, and the granularity of the activated carbon is 4-200 meshes; the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is Baotou rare earth concentrate.
B, dissolving the roasted Baotou rare earth concentrate by hydrochloric acid to obtain a chlorinated rare earth solution and acid leaching slag;
and step B, specifically, heating the roasted Baotou rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain a rare earth chloride solution and acid leaching slag.
The calcium content of the baotite is high, which affects the subsequent extraction and separation of rare earth, therefore, in the scheme, a step A0 is further included before the step A;
and A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate. That is, in this embodiment, the baotou rare earth concentrates are all baotou rare earth concentrates after calcium washing, and the CaO content of the baotou rare earth concentrates after calcium washing in this embodiment is 0.95%.
The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in this example was 52.73%.
Comparative experiment:
carrying out roasting experiments on Baotou rare earth concentrate raw ores without adding an active agent;
roasting a part of the Baotou rare earth concentrate raw ore obtained in the step A0 of the embodiment 1 at 800 ℃ for 2 hours; and then heating the product obtained after roasting to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, dissolving and leaching by using the hydrochloric acid, and filtering to obtain a rare earth chloride solution and acid leaching residues.
The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in the comparative experiment is 32.3%.
The roasted product in example 1, the roasted product in this comparative experiment, and the Baotou rare earth concentrate raw ore were analyzed, respectively, and the results are shown in Table 1;
wherein, TREO refers to the total content of rare earth oxide, P refers to the total content of phosphorus-containing oxide, and F refers to the total content of fluorine-containing oxide.
The roasted product A is a roasted product obtained by adding 15% of an active agent into Baotou rare earth concentrate and roasting; and the roasted product B is a roasted product obtained by directly roasting the calcium-washed Baotou rare earth concentrate raw ore.
TABLE 1 Baotou rare earth concentrate oxidizing roasting analysis report comparison table
Reason analysis: baotite is a mixed ore, and the ore contains rare earth phosphate and rare earth fluoride. After the calcium-washed raw ore is oxidized and roasted, 32.3% of rare earth can be leached out by hydrochloric acid. The leached part of rare earth should be lanthanum cerium carbon rare earth which is not combined with phosphorus and fluorine. When activated carbon is added for roasting, the activity of the rare earth element is improved under the action of the activator, so that the rare earth element is dissolved out by hydrochloric acid more, and the leaching rate of the rare earth is improved to 52.73%.
Comparative example 1
Comparison experiment of monazite ore:
this comparative example includes the following steps:
step one, roasting a part of monazite ore raw ore for 2 hours at 800 ℃;
step two: adding active carbon into the other part of the monazite ore raw ore, and uniformly mixing to obtain a material blending ore, wherein the adding amount of the active carbon is 15% of the mass of the monazite ore raw ore; the batch ore was then calcined at 800 ℃ for 2 hours.
And step three, heating the roasted products obtained in the step one and the step two to 95 ℃ by using 30% hydrochloric acid respectively, stirring for half an hour, dissolving by using the hydrochloric acid, leaching and filtering to obtain a rare earth chloride solution and acid leaching residues.
In this comparative example, the leaching rate of rare earth hydrochloric acid:
the leaching rate of the monazite ore raw ore is as follows: 0;
the leaching rate of the monazite ore added with the activated carbon is as follows: 0.57 percent.
The analysis report of the calcined product of this comparative example is shown in Table 2;
wherein, the roasted product D is a roasted product obtained by adding 15 percent of an active agent into monazite ores and roasting; the roasted product C is a roasted product obtained by directly roasting monazite ore raw ore.
TABLE 2 comparison table of monazite ore oxidizing roasting analysis report
Reason analysis shows that the monazite exists in the form of rare earth phosphate, the rare earth phosphate cannot be dissolved by hydrochloric acid by using an oxidizing roasting method, and the hydrochloric acid dissolution basically has no change after the activated carbon is added.
Comparative example 2
Comparative experiment against sichuan mine (flotation separation):
this comparative example includes the following steps:
step a, roasting a part of Sichuan ore at 800 ℃ for 2 hours.
And b, adding active carbon into the other part of Sichuan ore, wherein the adding amount of the active carbon is 15% of the mass of the raw Sichuan ore, so as to obtain a batch ore, and roasting the batch ore for 2 hours at 800 ℃.
And c, heating the roasted products obtained in the step a and the step b to 95 ℃ by using 30% hydrochloric acid respectively, stirring for half an hour, dissolving by using the hydrochloric acid, leaching, filtering, analyzing the content of the rare earth in the solution respectively, calculating the leaching rate (yield after adjustment) of the rare earth hydrochloric acid after the Sichuan ore raw ore is roasted and the Sichuan ore added with the activated carbon ore is roasted to obtain:
leaching rate of raw ore of Sichuan ore: 57.59 percent
Leaching rate of Sichuan ore added with activated carbon: 59.85 percent
The analysis report of the calcined product of this comparative example is shown in Table 3;
wherein the roasted product N is a roasted product obtained by adding 15% of an active agent into Sichuan ore and roasting; the roasted product M is a roasted product obtained by directly roasting raw ore of Sichuan ore.
TABLE 3 comparison table of the analytical report of the oxidation roasting of Sichuan mine
Reason analysis: the Sichuan ore exists in the form of rare earth fluoride and lanthanum-cerium-carbon which is not combined with fluorine, and the rare earth which is not combined with fluorine can be leached by hydrochloric acid by using an oxidizing roasting method. After the activator is added for roasting, the leaching rate of the rare earth is not obviously improved.
Example 2
This example is an example of no calcium washing before roasting Baotou rare earth concentrate:
a roasting method of rare earth ore concentrate added with an active agent comprises the following steps:
step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2 hours; the adding amount of the active agent is 15 percent of the mass of the rare earth concentrate;
the active agent is activated carbon, the granularity of the activated carbon is 4-200 meshes, the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is baotou rare earth concentrate after mineral separation.
B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag;
and step B, specifically, heating the roasted rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain a rare earth chloride solution and acid leaching slag.
In this example, the leaching rate (yield after adjustment) of rare earth hydrochloric acid was 65%.
Comparative experiment: carrying out roasting experiments on Baotou rare earth concentrates without adding an active agent;
roasting a part of Baotou rare earth concentrate raw ore with the same quality as the Baotou rare earth concentrate raw ore in the step A at the temperature of 800 ℃, wherein the roasting time is 2 hours; then, dissolving the roasted Baotou rare earth concentrate raw ore by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag; in the comparative experiment, the leaching rate (yield after adjustment) of rare earth hydrochloric acid for directly roasting Baotou rare earth concentrate raw ore is 45%.
Reason analysis: the baotite is a mixed ore, and the ore contains rare earth phosphate and rare earth fluoride; the CaO content in the raw ore is more than 7 percent, which is beneficial to improving the acid dissolution leaching rate of the rare earth, and the raw ore can be leached out 45 percent of the rare earth by hydrochloric acid after being oxidized and roasted. The leached part of rare earth should be lanthanum cerium carbon rare earth which is not combined with phosphorus and fluorine. When activated carbon is added for roasting, the activity of the rare earth element is improved under the action of the activator, so that more rare earth is dissolved by hydrochloric acid, and the leaching rate of the rare earth is improved to 65%. Since CaO affects the extraction process, the content of CaO needs to be controlled during actual production.
Example 3
A roasting method of rare earth ore concentrate added with an active agent comprises the following steps:
step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2 hours; the adding amount of the active agent is 15 percent of the mass of the rare earth concentrate;
wherein the active agent is activated carbon, and the granularity of the activated carbon is 4-200 meshes; the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is American ore rare earth concentrate.
B, dissolving the roasted American ore rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag;
and step B, specifically, heating the roasted American ore rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to finally obtain a rare earth chloride solution and acid leaching slag.
The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in this example was 61.36%.
Comparative experiment: roasting experiments are carried out on the raw ore of the American ore rare earth concentrate without adding the active agent;
roasting a part of the American ore rare earth concentrate raw ore with the same quality as that in example 3 at 800 ℃ for 2 hours; and then heating the product obtained after roasting to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, dissolving and leaching by using the hydrochloric acid, and filtering to obtain a rare earth chloride solution and acid leaching residues. The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in the comparative experiment is 50.3%.
Reason analysis: the american ore is also a mixed ore, similar to baotite, in which both rare earth phosphates and rare earth fluorides are present. When the raw ore is oxidized and roasted, 50.3% of rare earth can be leached out by hydrochloric acid. The leached part of rare earth should be lanthanum cerium carbon rare earth which is not combined with phosphorus and fluorine. When activated carbon is added for roasting, the activity of the rare earth element is improved under the action of the activator, so that more rare earth is dissolved by hydrochloric acid, and the leaching rate of the rare earth is improved to 61.36%.
Example 4
A roasting method of rare earth ore concentrate added with an active agent comprises the following steps:
step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 950 ℃, wherein the roasting time is 2.5 hours; the adding amount of the active agent is 15 percent of the mass of the rare earth concentrate;
the active agent is activated carbon, the granularity of the activated carbon is 4-200 meshes, the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is Baotou rare earth concentrate.
B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag;
and step B, specifically, heating the roasted rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain a rare earth chloride solution and acid leaching slag.
The calcium content of the baotite is high, which affects the subsequent extraction and separation of rare earth, therefore, in the scheme, a step A0 is further included before the step A;
and A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate.
Namely, calcium is washed from high-grade baotite rare earth ore, and the baotite rare earth concentrate is obtained by washing the calcium in the ore to be less than 1%.
The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in this example was 50%.
Example 5
A roasting method of rare earth ore concentrate added with an active agent comprises the following steps:
step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at the temperature of 600 ℃, wherein the roasting time is 1 hour; the adding amount of the active agent is 15 percent of the mass of the rare earth concentrate;
the active agent is activated carbon, the granularity of the activated carbon is 4-200 meshes, the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is Baotou rare earth concentrate.
B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag;
and step B, specifically, heating the roasted rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain a rare earth chloride solution and acid leaching slag.
The calcium content of the baotite is high, which affects the subsequent extraction and separation of rare earth, therefore, in the scheme, a step A0 is further included before the step A;
step A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the rare earth concentrate after calcium washing.
Namely, calcium is washed from high-grade baotite rare earth ore, and the baotite rare earth concentrate is obtained by washing the calcium in the ore to be less than 1%. In this example, the CaO content of the Baotou rare earth concentrate after calcium washing is 0.95%.
The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in this example was 46.5%.
Example 6
A roasting method of rare earth ore concentrate added with an active agent comprises the following steps:
step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2.5 hours; the adding amount of the active agent is 5 percent of the mass of the rare earth concentrate;
the active agent is activated carbon, the granularity of the activated carbon is 4-200 meshes, the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is Baotou rare earth concentrate.
B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag;
and step B, specifically, heating the roasted rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain a rare earth chloride solution and acid leaching slag.
The calcium content of the baotite is high, which affects the subsequent extraction and separation of rare earth, therefore, in the scheme, a step A0 is further included before the step A;
and A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate.
Namely, calcium is washed from high-grade baotite rare earth ore, and the baotite rare earth concentrate is obtained by washing the calcium in the ore to be less than 1%. In this example, the CaO content of the Baotou rare earth concentrate after calcium washing is 0.95%.
The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in this example was 43.56%.
Example 7
A roasting method of rare earth ore concentrate added with an active agent comprises the following steps:
step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 800 ℃, wherein the roasting time is 1 hour; the adding amount of the active agent is 30 percent of the mass of the rare earth concentrate;
the active agent is activated carbon, the granularity of the activated carbon is 4-200 meshes, the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is Baotou rare earth concentrate.
B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag;
and step B, specifically, heating the roasted rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain a rare earth chloride solution and acid leaching slag.
The calcium content of the baotite is high, which affects the subsequent extraction and separation of rare earth, therefore, in the scheme, a step A0 is further included before the step A;
and A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate.
Namely, calcium is washed from high-grade baotite rare earth ore, and the baotite rare earth concentrate is obtained by washing the calcium in the ore to be less than 1%. In this example, the CaO content of the Baotou rare earth concentrate after calcium washing is 0.95%.
The leaching rate (yield after adjustment) of the rare earth hydrochloric acid in this example was 50.7%.
Example 8
And A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate. In this example, the CaO content of the Baotou rare earth concentrate after calcium washing is 0.95%.
Step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2 hours; the adding amount of the active agent is 15 percent of the mass of the rare earth concentrate;
the active agent is activated carbon, the granularity of the activated carbon is 4-200 meshes, the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is Baotou rare earth concentrate.
B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag;
and step B, specifically, heating the roasted rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to finally obtain a rare earth chloride solution and acid leaching slag.
C, extracting the residual rare earth from the acid leaching residue obtained in the step B by using a sulfuric acid roasting process;
and C, adding concentrated sulfuric acid into the acid leaching residue obtained in the step B, adding the acid leaching residue into a rotary kiln, roasting at the temperature of about 850 ℃ to obtain roasted ore, leaching the roasted ore with water to obtain rare earth sulfate, and extracting and transforming the rare earth sulfate by p204 to obtain rare earth chloride solution.
In this embodiment, the leaching rate (yield after adjustment) of rare earth hydrochloric acid in the rare earth chloride solution obtained in step B is 52.7%; the rare earth yield of the sulfuric acid roasting method process in the step C is 94%.
Example 9
And A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate. In this example, the CaO content of the Baotou rare earth concentrate after calcium washing is 0.95%.
Step A, adding an active agent into the rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2 hours; the adding amount of the active agent is 15 percent of the mass of the rare earth concentrate;
the active agent is activated carbon, the granularity of the activated carbon is 4-200 meshes, the rare earth concentrate is rare earth mixed ore, and the rare earth mixed ore is Baotou rare earth concentrate.
B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag; and step B, specifically, heating the roasted rare earth concentrate to 95 ℃ by using 30% hydrochloric acid, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain a rare earth chloride solution and acid leaching slag.
C', removing fluorine and phosphorus from the acid leaching residue obtained in the step B by a sodium hydroxide alkali conversion method, dissolving by hydrochloric acid, and leaching rare earth;
specifically, adding sodium hydroxide into the acid leaching residue obtained in the step B, performing alkali conversion to obtain an alkali-converted ore, filtering, washing with water, adding hydrochloric acid with the concentration of 30% into the washed alkali-converted ore to dissolve, and leaching rare earth to obtain a rare earth chloride solution and an acid leaching residue.
The leaching rate (yield after adjustment) of rare earth hydrochloric acid of the chlorinated rare earth solution obtained in the step B is 52.7%;
in the step C', the rare earth yield is 85% by sodium hydroxide alkali-transfer method.
It should be noted that the lanthanum cerium carbon rare earth in the present invention refers specifically to the portion of rare earth elements that are not bonded with fluorine.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The roasting method of the rare earth ore concentrate added with the active agent is characterized by comprising the following steps:
step A, adding an active agent into rare earth concentrate, fully mixing, and roasting at the temperature of 600-950 ℃, wherein the roasting time is 0.5-2.5 hours;
the adding amount of the active agent is 5-30% of the mass of the rare earth concentrate;
the active agent is active carbon, and the rare earth concentrate is rare earth mixed ore.
2. The roasting method of rare earth ore concentrate added with an active agent according to claim 1, wherein the rare earth mixed ore is Baotou rare earth concentrate or American ore rare earth concentrate.
3. The roasting method of rare earth ore concentrate added with active agent according to claim 2, characterized by comprising the steps of:
step A, adding activated carbon into rare earth concentrate, fully mixing, and roasting at 800 ℃ for 2 hours;
the adding amount of the active agent is 15% of the mass of the rare earth concentrate;
the rare earth concentrate is Baotou rare earth concentrate.
4. The method for roasting active agent-added rare earth ore concentrate according to any one of claims 2 or 3, wherein the method for roasting active agent-added rare earth ore concentrate further comprises step B;
and step B, dissolving the roasted rare earth concentrate by hydrochloric acid to obtain a rare earth chloride solution and acid leaching slag.
5. The roasting method of rare earth ore concentrate added with active agent according to claim 4, wherein the particle size of the activated carbon is 4-200 meshes.
6. The method for roasting active agent-added rare earth ore concentrate according to claim 5, wherein the method for roasting active agent-added rare earth ore concentrate further comprises step C;
c, extracting the residual rare earth in the acid leaching residue by using the acid leaching residue obtained in the step B through a sulfuric acid roasting method process;
and C, adding concentrated sulfuric acid into the acid leaching residue obtained in the step B, adding the acid leaching residue into a rotary kiln, roasting at the temperature of about 850 ℃ to obtain roasted ore, leaching the roasted ore with water to obtain rare earth sulfate, and extracting and transforming the rare earth sulfate by p204 to obtain rare earth chloride solution.
7. The method for roasting active agent-added rare earth ore concentrate according to claim 5, wherein the method for roasting active agent-added rare earth ore concentrate further comprises the step C';
c', removing fluorine and phosphorus from the acid leaching residue obtained in the step B by a sodium hydroxide alkali conversion method, dissolving the acid leaching residue with hydrochloric acid, and leaching rare earth;
and C, adding sodium hydroxide into the acid leaching residue obtained in the step B, performing alkali conversion to obtain an alkali-converted ore, filtering, washing with water, adding hydrochloric acid into the washed alkali-converted ore to dissolve, and leaching rare earth to obtain a rare earth chloride solution and acid leaching residue.
8. The method for roasting active agent-added rare earth ore concentrate according to any one of claims 1 to 7, wherein the method for roasting active agent-added rare earth ore concentrate further comprises step A0;
and A0, washing calcium from the high-grade rare earth ore, and washing the calcium in the ore to be less than 1% to obtain the calcium-washed rare earth concentrate.
9. The roasting method of rare earth ore concentrate added with active agent according to claim 8, characterized in that the step B comprises the following steps: adding hydrochloric acid with the concentration of 30% into the roasted rare earth concentrate, heating to 95 ℃, stirring for 0.5 hour, cooling, standing, extracting supernatant and feed liquid with slag, and filtering to obtain rare earth chloride solution and acid leaching slag.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013139617A (en) * | 2012-01-06 | 2013-07-18 | Hitachi Ltd | Method for separating and recovering rare earth element |
| CN104404243A (en) * | 2014-12-12 | 2015-03-11 | 钢研集团稀土科技有限公司 | Method for low-temperature decomposition of low-grade Weishan rare earth ore concentrate through acid-alkali combination |
| CN109136590A (en) * | 2018-09-20 | 2019-01-04 | 甘肃稀土新材料股份有限公司 | A kind of packet header mixed rare earth concentrate decomposition processing process |
| CN112074617A (en) * | 2019-11-20 | 2020-12-11 | 包头稀土研究院 | Smelting method of bastnaesite and application of carbon powder |
-
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- 2022-04-24 CN CN202210434414.XA patent/CN114752788A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013139617A (en) * | 2012-01-06 | 2013-07-18 | Hitachi Ltd | Method for separating and recovering rare earth element |
| CN104404243A (en) * | 2014-12-12 | 2015-03-11 | 钢研集团稀土科技有限公司 | Method for low-temperature decomposition of low-grade Weishan rare earth ore concentrate through acid-alkali combination |
| CN109136590A (en) * | 2018-09-20 | 2019-01-04 | 甘肃稀土新材料股份有限公司 | A kind of packet header mixed rare earth concentrate decomposition processing process |
| CN112074617A (en) * | 2019-11-20 | 2020-12-11 | 包头稀土研究院 | Smelting method of bastnaesite and application of carbon powder |
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