KR102109623B1 - Method for manufacturing rare earth magnetic powder from monazite - Google Patents

Abstract

The present invention comprises the steps of preparing an intermediate solution containing Nd and Pr; Mixing the intermediate product solution and a Fe source material to prepare a magnetic material solution in which magnetic materials including Nd, Pr, and Fe are dissolved; Preparing a magnetic material hydroxide from the magnetic material solution by coprecipitation; Heating the magnetic material hydroxide to produce a magnetic material oxide; Adding an additive to the magnetic material oxide; Reducing and diffusing the magnetic material oxide to which the additive is added to prepare magnetic powder; And washing the magnetic powder, wherein the preparing of the intermediate product solution comprises: sulfating the rare earth concentrate monazite with sulfuric acid; Water-leaching the reaction product after the sulfation reaction; Precipitating the rare earth element by adding sodium sulfate after the water leaching; And a solvent extraction of the precipitated rare earth elements; to obtain an intermediate product solution by precipitation and solvent extraction of the rare earth elements, wherein the magnetic material in the magnetic material solution is in a chloride state, and the magnetic material solution. Relates to a method for producing rare earth magnetic powder from monazite further comprising at least one additional magnetic material selected from the group consisting of Dy source material, Nd source material, Co source material, and Y source material.

Description

Method for manufacturing rare earth magnetic powder from monazite}

The present invention relates to a method for producing rare earth magnetic powder from monazite.

The permanent magnet is a material that retains the magnetic field in the material even when the externally applied magnetic field is removed, and is essentially used for motors, generators, and electronic devices.

Recently, as energy reduction and environment-friendly green growth projects are rapidly emerging as new issues, technological demand for rare earth permanent magnets that show energy efficiency improvement is increasing due to excellent light magnetic performance.

As a permanent magnet material exhibiting such excellent magnetic performance, an R-Fe-B-based rare earth magnet is known.

However, in order to manufacture rare earth magnets, magnetic powder must be prepared. In the existing magnetic powder manufacturing method, the magnetic force properties (coercive force, etc.) of the produced magnetic powder are reduced due to defects in magnetic properties such as mechanical residual stress, etc. As the defect effect was further increased, there was a quality problem that the characteristics became unstable.

In addition, in manufacturing rare earth magnets, expensive rare earth elements are used as the main raw material, so manufacturing cost is higher than that of ferrite magnets, which increases the burden of price increase, as well as the resource limitations of rare earth elements that are not rich compared to other metals. There is.

In order to secure such a rare earth element, in recent years, a method of extracting a rare earth element from a rare earth concentrate and producing it as a magnetic powder has been attempted.

However, the above methods for manufacturing magnetic powder from rare earth concentrates require high temperature, fine control of pressure and pH, and there is a problem in that it is not easy to extract rare earth and manufacture magnetic powder through it.

Republic of Korea Registered Patent Publication No. 10-1261099 (registered on April 29, 2013)

The present invention is to solve the above problems, to provide a method for producing a rare-earth magnetic powder from the monazite excellent magnetic force properties of the magnetic powder.

The present invention comprises the steps of preparing an intermediate solution containing Nd and Pr; Mixing the intermediate product solution and a Fe source material to prepare a magnetic material solution in which magnetic materials including Nd, Pr, and Fe are dissolved; Preparing a magnetic material hydroxide from the magnetic material solution by coprecipitation; Heating the magnetic material hydroxide to produce a magnetic material oxide; Adding an additive to the magnetic material oxide; Reducing and diffusing the magnetic material oxide to which the additive is added to prepare magnetic powder; And it provides a method for producing a rare earth magnetic powder from monazite comprising the step of washing the magnetic powder.

The step of preparing the intermediate product solution includes the steps of sulfated monazite, a rare earth concentrate, using sulfuric acid; Water-leaching the reaction product after the sulfation reaction; Precipitating the rare earth element by adding sodium sulfate after the water leaching; And solvent extraction of the precipitated rare earth elements; and an intermediate solution may be obtained by precipitation of the rare earth elements and solvent extraction.

The sulfuric acid is added in a weight ratio of 0.1 to 0.7 relative to the total amount of monazite, the sulfation reaction is performed at 180 to 220 ° C for 1 to 3 hours, and the water leaching is performed at 30 to 80 ° C for 100 to 150 minutes, , The sodium sulfate may be added in an amount of 1.8 to 2.2 equivalents with respect to the rare earth element.

In the magnetic material solution, the magnetic material is in a chloride state, and the magnetic material solution may further include at least one additional magnetic material selected from the group consisting of Dy source material, Nd source material, Co source material, and Y source material. have.

The magnetic material solution may further include a Dy source material as the additional magnetic material.

The coprecipitation may be performed by adjusting the acidity of the magnetic material solution.

The acidity adjustment is performed by adding NaOH to the magnetic material solution, and the acidity can be adjusted to 13 or more.

The manufacturing of the magnetic material oxide may include: desalting the magnetic material hydroxide; And after the desalting step of drying for 8 to 10 hours at 100 ~ 110 ℃; further comprises, the heating may be performed for 30 minutes ~ 2 hours at 700 ~ 1000 ℃ after drying.

The additive may include a boron source material and a calcium source material.

The boron source material may include H ₃ BO ₃ , and the calcium source material may include CaH ₂ .

The mass ratio of the magnetic material oxide and the calcium source material may be 1: 0.7 to 1.2.

The magnetic powder may include Nd, Pr, Fe and B.

The magnetic powder preparation may be performed in an argon atmosphere through heat treatment at 600 to 1000 ° C for 1 to 3 hours.

The washing of the magnetic powder may include washing by adding at least one of purified water and acetone to the magnetic powder; And drying under reduced pressure for 1 to 4 hours.

From the monazite of the present invention, it is possible to manufacture a magnetic powder having a remarkably increased magnetic force characteristic according to a method for producing a rare-earth magnetic powder.

1 is a flow chart showing a method of manufacturing a rare earth magnetic powder from monazite according to an embodiment of the present invention,
Figure 2 is the XRD analysis results in [Experimental Example 1] according to the concentration change of the intermediate product solution,
3 is a VSM result in [Experimental Example 1] according to the concentration change of the intermediate solution,
Figure 4 is a SEM photograph showing the particle distribution of the magnetic powder element according to [Experimental Example 1],
5 is an XRD analysis result in [Experimental Example 2] in which the additive Dy source material was added to the intermediate product solution,
6 is a VSM result in [Experimental Example 2] according to the concentration change of the intermediate product solution after the additive Dy source material is added,
7 is a VSM result in [Experimental Example 3] according to the additional addition of the additive Nd source material to the intermediate solution,
8 is an XRD analysis result in [Experimental Example 4] according to additional addition of an additive Co source material and a Y source material to the intermediate product solution,
9 is a VSM result in [Experimental Example 4] according to the addition of the additive Co source material and Y source material to the intermediate solution.

Advantages and features of the present invention, and a method of achieving the advantages and features will be apparent with reference to the embodiments described below with reference to the accompanying drawings.

However, the present invention will not be limited to the embodiments disclosed below, but will be implemented in various different forms, and only the present embodiments allow the disclosure of the present invention to be complete, and common knowledge in the art to which the present invention pertains. It is provided to completely inform the person having the scope of the invention, and the present invention is only defined by the scope of the claims.

In addition, in the description of the present invention, if it is determined that related known technologies may obscure the subject matter of the present invention, detailed descriptions thereof will be omitted.

1 is a flow chart showing a method of manufacturing a rare earth magnetic powder from monazite according to an embodiment of the present invention.

Referring to FIG. 1, first, an intermediate solution containing Nd and Pr is prepared from monazite, a rare earth concentrate. (S1, S2, S3)

In this step, the rare earth concentrate is sulfated using sulfuric acid. (S1)

When sulfuric acid is used for the rare earth concentrate, monazite, a sulfation reaction as shown in Reaction Scheme 1 below occurs.

[Scheme 1]

REPO ₄ + 3H ₂ SO ₄ → RE ₂ (SO ₄ ) ₃ + 3H ₃ PO ₄ (RE = La, Ce, Pr or Nd, etc.)

Sulfuric acid can be added in a weight ratio of 0.1 to 0.7 based on the total amount of rare earth concentrate.

The sulfation reaction can be performed at 180 to 220 ° C. for 1 to 3 hours. When the sulfation reaction temperature is too low, the rare earth concentrate and sulfuric acid sulfation reaction occurs insufficiently, resulting in a problem that the amount of rare earth elements leached upon water leaching occurs, and when the temperature is too high, sulfuric acid decomposes and sulfates The problem that the reaction is lowered occurs.

After the sulfation reaction, the reaction product is leached with water (S2).

The rare earth element is leached from the rare earth concentrate, monazite, by sulfuric acid reaction with sulfuric acid, followed by leaching of the reaction product.

When leaching water, the concentration of the mineral solution in the rare earth concentrate may be 10 to 50% by weight.

When the concentration of the mineral solution is less than 10% by weight, the leaching rate of the rare earth elements is high, but the concentration of the rare earth in the recovered leaching solution is low, resulting in a problem that the efficiency of the process decreases, and when it exceeds 50% by weight, A problem that the leaching rate decreases occurs.

Water leaching can be performed at 30-80 ° C. for 100-150 minutes.

When the temperature of water leaching is less than 30 ° C, a problem occurs in which the leaching rate of rare earth concentrates is lowered, and when it exceeds 80 ° C, a problem that the leaching rate is not significantly improved even when the temperature increases.

After water leaching, sodium sulphate is added to precipitate rare earth elements, and the solvent is extracted to prepare an intermediate solution. (S3)

In the leach solution after water leaching, rare earth elements separated from monazite, which is a rare earth concentrate, exist, and when sodium sulfate is added, a rare earth-sodium sulfate double salt precipitation reaction occurs to precipitate rare earth elements.

[Scheme 2]

RE ₂ (SO ₄ ) ₃ + Na ₂ SO ₄ → 2RE · NA (SO ₄ ) ₂ ↓ (RE = La, Ce, Pr or Nd, etc.)

Sodium sulfate is added in an amount of 1.8 to 2.2 equivalents based on rare earth elements. When sodium sulfate is added in an amount of less than 1.8 equivalents, a problem occurs in that the recovery rate of rare earth elements is lowered, and when it is added in excess of 2.2 equivalents, a problem in that the recovery rate of rare earth elements is no longer increased.

Precipitation of rare earth elements can be performed at 40-60 ° C. for 1-2 hours. When the rare earth element is precipitated, when the reaction temperature is less than 40 ° C, a problem occurs in that the recovery rate of the rare earth element is lowered, and when it exceeds 60 ° C, the recovery rate of the rare earth element does not increase any more.

Mixed rare earth double salts selectively precipitated with sodium sulfate are converted to mixed rare earth hydroxides with caustic soda, washed with water to remove other impurities, and calcined at 900 ° C to prepare mixed rare earth oxides.

A mixed rare-earth chloride solution is prepared so that the rare-earth oxide is leached in an appropriate concentration (1.0-2.0M) hydrochloric acid to have a rare-earth concentration of 0.5-1.0M, and a 0.5-1.0M phosphate-based extractant (2-Ethylhexyl 2-ethylhexyphosphonic acid) Etc.) to extract and remove rare earth components with higher atomic numbers than samarium, which has a high tendency to extract.

After extraction containing only La, Ce, Pr, and Nd components, the pH of the filtrate is adjusted with 0.5 ~ 1.0M phosphate-based extractant (2-Ethylhexyl 2-ethylhexyphosphonic acid, etc.), separated from La and Ce components And extracts only Pr and Nd components.

Then, the Pr and Nd components extracted by the extractant are removed with hydrochloric acid to prepare an intermediate product solution containing only the Pr and Nd components.

Through the precipitation and solvent extraction step (S3), an intermediate solution containing rare earth elements Nd and Pr is prepared.

Next, the intermediate material solution and the Fe source material are mixed to prepare a magnetic material solution in which magnetic materials including Nd, Pr, and Fe are dissolved. (S4)

When the intermediate product solution and the Fe source material are mixed, a magnetic material solution in which magnetic materials including Nd, Pr, and Fe are dissolved can be obtained. In the magnetic material solution, the magnetic material may be in a chloride state.

The Fe source material may include FeCl ₂ .

In this step, one or more additional magnetic materials selected from the group consisting of Dy source material, Nd source material, Co source material, and Y source material may be further added to the magnetic material solution.

Additional magnetic materials can also be added in the form of chlorides, and magnetic properties (coercive force) can be improved by adding magnetic materials.

The effect of magnetic properties (coercive force) due to the addition of the additional magnetic material as described above will be described later.

Next, a magnetic material hydroxide is prepared from a magnetic material solution by coprecipitation. (S5)

Coprecipitation in the present invention can be performed by adjusting the acidity of the magnetic material solution, and by adding NaOH to the magnetic material solution to adjust the acidity to 13 or more.

Thereafter, the magnetic material hydroxide is heated to prepare a magnetic material oxide. (S6)

In order to manufacture the magnetic material oxide, the magnetic material hydroxide may be desalted, and after desalting, a drying and heating step may be performed.

Desalination can remove NaCl in the magnetic hydroxide by washing with purified water and ethanol.

After desalting, drying is performed at 100 to 110 ° C for 8 to 10 hours, and heating can be performed at 700 to 1000 ° C for 30 minutes to 2 hours after drying.

When the magnetic material hydroxide generated by coprecipitation of the magnetic material solution containing the Fe source material is desalted, and then dried and heated after desalting, a magnetic material oxide is obtained as shown in Reaction Scheme 3 below.

[Scheme 3]

RE (OH) ₃ + Fe (OH) ₃ → FeREO ₃ + Fe ₃ O ₄ + Fe ₂ O ₃ (RE = Nd and Pr)

Next, an additive is added to the magnetic material oxide. (S7)

As an additive, a boron source material and a calcium source material may be added, and the boron source material may include H ₃ BO ₃ and / or B ₂ O ₃ .

In the present invention, the calcium source material serving as a reducing agent is Ca or CaH _2, CaCl ₂ , Ca (OH) ₂ , CaCO ₃ , Ca (NO ₃ ) 2 · 4H ₂ O, Ca (CH ₃ COO) 2 · H _It may be at least one material selected from the group consisting of ₂ O and CaSO ₄ · 2H ₂ O.

In the present invention, the mass ratio of the magnetic material oxide and the calcium source material is preferably 1: 0.7 to 1.2, and more preferably, the mass ratio of the magnetic material oxide and the calcium source material is 1: 0.9 to 1: 1.1. Do.

Next, the magnetic material oxide to which the additive is added is reduced and diffused to prepare a magnetic powder. (S8)

Reduction diffusion can be carried out by heat treatment for 1 to 3 hours at 600 to 1000 ° C under argon atmosphere or vacuum atmosphere, and magnetic powder generated by diffusion diffusion of magnetic material oxides includes Nd, Pr, Fe and B. Can be.

In addition, the magnetic powder may further include Dy, Nd, Co, and Y, which are additional magnetic materials added in step S4 of preparing a magnetic material solution.

When the process temperature is less than 600 ° C, the added calcium source material does not melt, so the fluidity for reduction or diffusion may be insufficient, and when the process temperature exceeds 1000 ° C, particle growth may occur, which is not preferable.

Finally, the prepared magnetic powder is washed (S9).

The washing step of the magnetic powder can be prepared by adding at least one of purified water and acetone to the magnetic powder, followed by drying for 1 to 4 hours under reduced pressure to produce the final powder.

The magnetic component powder finally produced according to the method for manufacturing rare earth magnetic component powder from the monazite of the present invention does not deteriorate the magnetic force characteristics, and makes it possible to produce a magnetic component powder having a significantly increased coercive force characteristic.

Hereinafter, experimental examples of the present invention will be described in detail with reference to the accompanying drawings.

[Experimental Example 1]

400 g of Monazite concentrate of Samcheon-gun, Hwanghaenam-do, North Korea was sulfated by using 120 g of sulfuric acid. At this time, the sulfation reaction temperature was 200 ° C, and the reaction time was performed for 2 hours. After the sulfation reaction, the reaction product was leached into water, wherein the monazite mineral solution concentration was 20% by weight, and the leaching temperature was performed at 60 ° C for 120 minutes.

After the leaching of water, sodium sulfate was added to the leaching solution to precipitate the rare earth elements contained in the leaching solution, and the precipitated rare earth elements were mixed with hydroxide, prepared by mixing with a rare earth oxide by water washing and firing, and then leached with hydrochloric acid to phosphate. Only the Pr and Nd components were recovered by the system extractant to prepare an intermediate solution.

After water leaching, sodium sulfate was added to the leaching solution to precipitate rare earth elements contained in the leaching solution, and the precipitated rare earth elements were recovered as a leaching solution to prepare an intermediate product solution containing Nd and Pr.

The Fe source material FeCl ₂ was mixed with the intermediate product solution to prepare a magnetic material solution in which magnetic materials including Nd, Pr, and Fe were dissolved.

Thereafter, 3.5 g / mol of NaOH was added to the magnetic material solution to adjust the acidity to 13 or higher, and coprecipitation was performed at 180 rpm on a stirring plate for 4 hours to prepare a magnetic material hydroxide.

Next, the magnetic material hydroxide was washed twice with purified water and once with ethanol to perform a desalting process to remove NaCl generated during coprecipitation.

After desalting, the mixture was dried at 110 ° C for 9 hours, and then dried and heated at 700 ° C for 30 minutes to prepare a magnetic material oxide.

H ₃ BO ₃ as an additive to the prepared magnetic oxide and CaH ₂ was added, and a pressure of 10 Mpa was applied for 2 minutes, and the magnetic material oxide was mixed until it became a pellet. At this time, the mixing ratio of the magnetic material oxide and CaH ₂ was adjusted to be 1: 1.

Additive H₃BO₃And CaH₂The added magnetic material oxide was heat treated at 1000 ° C. for 3 hours in an argon atmosphere and then subjected to diffusion diffusion treatment, followed by washing with purified water or acetone. Ultrasonics were used to completely dissolve impurities during cleaning.

After washing, the final magnetic powder was prepared by drying under reduced pressure for 4 hours.

In the magnetic powder prepared according to Experimental Example 1 of the present invention, magnetic properties of magnetic powder according to the concentration of the intermediate product solution containing Nd and Pr are shown through Table 1 and FIGS. 2 to 4.

2 is a result of XRD analysis in [Experimental Example 1] according to the concentration change of the intermediate product solution, FIG. 3 is a result of VSM in [Experimental Example 1] according to the concentration change of the intermediate product solution, and FIG. 4 is [Experiment] Example 1] is a SEM photograph showing the particle distribution of magnetic powder elements.

RE (Nd-Pr) Hc (k Oe.) Mr (emu / g) BHmax (MGOe) 5.0 4.07 53.50 2.41 8.2 4.54 53.80 2.93 10.0 4.07 47.50 2.09 15.0 2.00 21.40 0.39

[Table 1] shows that the concentration of RE (Nd / Pr) is 8.2 when the magnetic properties of the magnetic powder are maximum according to the concentration change of the intermediate solution.

The maximum energy (BHmax), coercive force (Hc), and magnetization (Mr) values according to the concentration change indicate the maximum value when the content of RE (Nd / Pr) in the intermediate product solution is 8.2. It can be seen that the magnetic properties of the magnetic powder change according to the concentration change of the intermediate solution.

2 is an XRD analysis result in [Experimental Example 1] according to the concentration change of the intermediate product solution.

Referring to Figure 2, it can be confirmed that a large amount of Fe ₂ Pr and Nd was detected in the magnetic powder prepared according to [Experimental Example 1]. That is, it can be seen that the magnetic powder according to the manufacturing method of [Experimental Example 1] contains added additives Fe and B, and contains a large amount of Nd and Pr.

3 is a VSM result in [Experimental Example 1] according to the concentration change of the intermediate solution.

As shown in [Table 1], it can be seen that the magnetic properties of the magnetic powder according to the concentration change of the intermediate product solution shows the maximum value when the RE (Nd / Pr) content in the intermediate product solution is 8.2.

The RE (Nd / Pr) content in the intermediate solution was 8.2 days, the coercive force (Hc) was 4.54 k Oe., The magnetization (Mr) was 53.80 emu / g, and the maximum energy (BHmax) was 2.93 MGOe.

Figure 4 is a SEM photograph showing the particle distribution of the magnetic powder element according to [Experimental Example 1].

4 is a SEM of the distribution of component elements when the content of RE (Nd / Pr) in the intermediate product solution is 8.2, as shown in [Table 1], among the manufacturing methods of the final magnetic powders prepared through [Experimental Example 1]. Through.

Referring to FIG. 4, it can be confirmed that in the distribution state of the component elements of the final powder, the main element Fe and the rare earth elements Nd and Pr show a uniform distribution.

[Experimental Example 2]

In the process of preparing rare earth magnetic powder from monazite according to the manufacturing method of [Experimental Example 1], an additive Dy source material was further added to the intermediate product solution containing Nd and Pr, and the rest of the process was performed in the same manner.

5 is an XRD analysis result in [Experimental Example 2] in which the additive Dy source material was added to the intermediate solution.

Referring to Figure 5, it can be confirmed that a large amount of Dy was detected in the magnetic powder prepared according to [Experimental Example 2]. That is, the magnetic powder according to the manufacturing method of [Experimental Example 2] includes Fe, B, Nd, and Pr, and it can be confirmed that the added additive Dy is contained in a large amount.

6 is a VSM result in [Experimental Example 2] according to the concentration change of the intermediate product solution after the addition of the additive Dy source material.

As shown in FIG. 6, it was confirmed that the magnetic properties of the magnetic powder according to the concentration change of the intermediate product solution after the addition of the additive Dy source material shows the maximum value when the content of RE (Nd / Pr) in the intermediate product solution is 8. Can be.

When the additive Dy in the intermediate solution was added, it was confirmed that the magnetic properties were improved by increasing the coercive force (Hc), magnetization (Mr), and maximum energy (BHmax) when the RE (Nd / Pr) content was 8 Can be.

[Experimental Example 3]

In the process of preparing rare earth magnetic powder from monazite according to the preparation method of [Experimental Example 1], Nd source material, which is an additive, was further added to the intermediate product solution containing Nd and Pr, and the rest of the process was performed in the same manner.

7 is a VSM result in [Experimental Example 3] according to the additional addition of the additive Nd source material to the intermediate solution.

As illustrated in FIG. 7, when Nd and Pr are further added to Nd, the magnetic properties are increased when the composition ratio of Pr is relatively lowered, that is, when the Nd composition ratio in the intermediate solution is adjusted larger. can confirm.

In other words, it can be confirmed that Pr, when present together with Nd, shows a result of deteriorating magnetic properties more than when Nd is present alone.

Referring to FIG. 7, when the additive Nd in the intermediate solution is further added, and the content of RE (Nd / Pr) in the intermediate solution is the same, the coercive force (Hc), magnetization (Mr), and maximum energy (BHmax) It can be seen that the magnetic properties are improved when the composition ratio of Pr is relatively lowered by adding Nd.

[Experimental Example 4]

In the process of preparing rare earth magnetic powder from monazite according to the manufacturing method of [Experimental Example 1], the additive Co source material and the Y source material were further added to the intermediate product solution containing Nd and Pr, and the rest of the process was performed in the same manner. Did.

8 is an XRD analysis result in [Experimental Example 4] according to additional addition of an additive Co source material and a Y source material to the intermediate solution.

Referring to Figure 8, it can be confirmed that only a small amount of Co was detected in the magnetic powder prepared according to [Experimental Example 4]. That is, the magnetic powder according to the manufacturing method of [Experimental Example 4] includes Fe, B, Nd, Pr, and Co, and it can be seen that only a small amount of the additive Co is added.

9 is a VSM result in [Experimental Example 4] according to the addition of the additive Co source material and Y source material to the intermediate solution.

As shown in FIG. 9, the contents of RE (Nd / Pr) in the intermediate solution are the same, and it can be confirmed that the magnetic properties of the magnetic powder are not significantly improved even when the additive Co source material and the Y source material are further added. .

The coercive force (Hc) in the case of the magnetic powder with additional additives Co source material and Y source material added, compared to the magnetic powder with additive Dy added in the intermediate product solution prepared according to the manufacturing method in [Experimental Example 2] , It can be confirmed that there is little change in magnetization (Mr) and maximum energy (BHmax), and there is no improvement in magnetic properties.

Although the embodiments of the present invention have been described with reference to the above and the accompanying drawings, those of ordinary skill in the art to which the present invention pertains can implement the present invention in other specific forms without changing its technical spirit or essential features. You will understand that there is. Therefore, it should be understood that the embodiments described above are illustrative in all respects and not restrictive.

Claims (14)

Preparing an intermediate solution containing Nd and Pr;
Mixing the intermediate product solution and a Fe source material to prepare a magnetic material solution in which magnetic materials including Nd, Pr, and Fe are dissolved;
Preparing a magnetic material hydroxide from the magnetic material solution by coprecipitation;
Heating the magnetic material hydroxide to produce a magnetic material oxide;
Adding an additive to the magnetic material oxide;
Reducing and diffusing the magnetic material oxide to which the additive is added to prepare magnetic powder; And
And cleaning the magnetic powder.
The step of preparing the intermediate product solution,
Sulfurizing rare earth concentrate monazite using sulfuric acid;
Water-leaching the reaction product after the sulfation reaction;
Precipitating the rare earth element by adding sodium sulfate after the water leaching; And
Includes; the solvent extraction of the precipitated rare earth elements;
Intermediate solution is obtained by precipitation of the rare earth element and solvent extraction,
In the magnetic material solution, the magnetic material is in a chloride state,
The magnetic material solution further includes at least one additional magnetic material selected from the group consisting of Dy source material, Nd source material, Co source material, and Y source material,
The coprecipitation is performed by adjusting the acidity of the magnetic material solution, and adjusting the acidity is adjusted to an acidity of 13 or more by adding NaOH to the magnetic material solution,
The step of manufacturing the magnetic material oxide,
A desalting step of washing the magnetic material hydroxide with purified water and ethanol to remove NaCl generated during the coprecipitation; And
After the desalting step of drying for 8 to 10 hours at 100 ~ 110 ℃; further comprises,
The heating is performed for 30 minutes to 2 hours at 700 to 1000 ° C after the drying,
The additive comprises boron source material H ₃ BO ₃ , calcium source material CaH ₂ ,
The step of washing the magnetic powder,
Adding at least one of purified water and acetone to the magnetic powder and washing using ultrasonic waves; And
Drying for 1-4 hours under reduced pressure; Method for producing rare earth magnetic powder from monazite containing. delete In claim 1,
The sulfuric acid is added in a weight ratio of 0.1 to 0.7 with respect to the total amount of monazite,
The sulfate reaction is carried out at 180 ~ 220 ℃ for 1 to 3 hours,
The water leaching is performed at 30 ~ 80 ℃ for 100 ~ 150 minutes,
The sodium sulfate is a method for producing a rare earth magnetic powder from monazite, characterized in that it is added in an amount of 1.8 to 2.2 equivalents relative to the rare earth element. delete In claim 1,
The magnetic material solution is a method for producing a rare earth magnetic powder from monazite, characterized in that it further comprises a Dy source material as the additional magnetic material. delete delete delete delete delete In claim 1,
A method for producing a rare earth magnetic powder from monazite, wherein the mass ratio of the magnetic material oxide and the calcium source material is 1: 0.7 to 1.2. In claim 1,
The magnetic powder is Nd, Pr, Fe and method for producing a rare earth magnetic powder from monazite, characterized in that it comprises B. In claim 1,
The magnetic powder manufacturing,
Method of manufacturing rare earth magnetic powder from monazite, characterized in that it is performed through heat treatment at 600 to 1000 ° C for 1 to 3 hours in an argon atmosphere. delete

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