CN115449624A - Method for treating high-iron low-phosphorus rare earth ore - Google Patents

Method for treating high-iron low-phosphorus rare earth ore Download PDF

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CN115449624A
CN115449624A CN202210959394.8A CN202210959394A CN115449624A CN 115449624 A CN115449624 A CN 115449624A CN 202210959394 A CN202210959394 A CN 202210959394A CN 115449624 A CN115449624 A CN 115449624A
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rare earth
iron
ore
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phosphorus
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孟玉琴
李虎平
王维欢
李向东
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Gansu Rare Earth New Material LLC
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Gansu Rare Earth New Material LLC
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • C22B1/06Sulfating roasting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00Obtaining rare earth metals
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention discloses a method for treating high-iron low-phosphorus rare earth ore, belonging to the technical field of rare earth ore production, comprising the process of high-temperature reinforced roasting by concentrated sulfuric acid of rare earth concentrate, wherein before the roasting by adding the concentrated sulfuric acid, high-iron low-phosphorus rare earth ore accounting for 10-15% of the total ore mass is also added into the rare earth concentrate, and the rare earth occurrence structures of the high-iron low-phosphorus rare earth ore and the rare earth concentrate are phosphoric acid rare earth. According to the invention, the iron powder in the original process is partially or completely replaced by the high-iron low-phosphorus rare earth ore, so that the consumption of the iron powder is reduced, the utilization rate of the high-iron low-phosphorus rare earth ore is increased, the defect of poor concentrate composition is compensated at low cost, the leaching rate of the rare earth is stabilized to be more than 96%, two defective rare earth ores can be fully utilized, and the technical problem that the defective rare earth ore cannot be effectively treated at low cost in the prior art is solved.

Description

Method for treating high-iron low-phosphorus rare earth ore
Technical Field
The invention belongs to the technical field of rare earth ore production, and particularly relates to a method for treating high-iron low-phosphorus rare earth ore.
Background
China is a big country of rare earth ores, has rich rare earth ore resources, and then the rare earth ores occupying a certain proportion have the following problems: firstly, the grade is too low, the grade of the rare earth ore with high iron and low phosphorus is generally about 20%, the rare earth ore cannot be processed as normal rare earth ore due to low grade, and the yield is low even if the rare earth ore is processed. Secondly, the components are not good, in recent years, the content of phosphate radicals in baotite concentrates is 17% -19%, the average content of iron oxide is only about 2-3%, for example, rare earth ores in baotite regions mainly comprising bastnaesite and monazite, the iron-phosphorus ratio in water extract after roasting by sulfuric acid is far less than 3 due to the components, the yield of rare earth is reduced after neutralization and impurity removal, and the yield of rare earth of the process is influenced, so that the yield is improved by adding Fe as a phosphorus fixing agent to generate ferric pyrophosphate. Through a large number of scientific experiments and production practices, the unit consumption of iron powder in the prior art is generally 25-30% of the quality of baotian concentrate, and accounts for about 12-20% of the total concentrate decomposition cost, so that the production cost is increased, and the development of the industry is influenced. Therefore, the development of a method for fully utilizing the rare earth ore with the defects is a necessary way for the development of the rare earth industry and is also a necessary way for whether the rare earth resources can be fully utilized in China.
Disclosure of Invention
The invention aims to provide a method for treating high-iron low-phosphorus rare earth ore, which solves the technical problem that the prior art cannot effectively treat defective rare earth ore at low cost.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for processing high-iron low-phosphorus rare earth ore comprises a high-temperature reinforced roasting process of concentrated sulfuric acid of rare earth ore concentrate, wherein before the roasting process of the concentrated sulfuric acid, high-iron low-phosphorus rare earth ore accounting for 10-15% of the total ore mass is added into the rare earth ore concentrate, and rare earth occurrence structures of the high-iron low-phosphorus rare earth ore and the rare earth ore concentrate are phosphoric acid rare earth.
Preferably, the adding amount of the concentrated sulfuric acid is 1.5 to 1.7 times of the total mass of the high-iron low-phosphorus rare earth ore and the rare earth concentrate.
Further, the method comprises the following steps:
(1) Adding high-iron low-phosphorus rare earth ore into the rare earth concentrate, and uniformly mixing;
(2) Adding concentrated sulfuric acid into the mixed ore, uniformly mixing, placing the mixture into a high-temperature box type furnace, roasting at the low temperature of 280-300 ℃ for 60-120 min, then raising the temperature in the furnace to 400-420 ℃ until the fluid material is completely solidified, discharging, turning and crushing by using a small shovel, returning the material to the high-temperature box type furnace, continuously roasting for 30-60 min, discharging, and turning and crushing by using the small shovel; returning the materials to the high-temperature box furnace again to continue roasting for 30-60 min, stopping the furnace, grinding the sample by using a sampling machine after the temperature is reduced, sieving the sample by using a sieve, and adding magnesium sulfate water to leach for 2h;
(3) And (3) size mixing, filter pressing, neutralizing the filtrate and carrying out filter pressing again to obtain the rare earth leaching solution.
Preferably, in the step (1), iron powder accounting for 0-15% of the mass of the rare earth concentrate is also added.
More preferably, in the step (2), the screen is a 200-mesh screen.
Preferably, in the step (3), the filter residue obtained by filter pressing after size mixing is subjected to slag washing and filter pressing, the filtrate obtained by slag washing is returned to the size mixing process to be used as a liquid phase, and the filter residue obtained by slag washing is discharged after being soaked again.
Preferably, in the step (3), the filter residue obtained by neutralization is returned to the size mixing procedure to be treated again as a solid phase.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, iron powder in the original process is partially or completely replaced by the high-iron low-phosphorus rare earth ore, so that the consumption of the iron powder is reduced, the utilization rate of the high-iron low-phosphorus rare earth ore is improved, the defect of poor concentrate composition is compensated at low cost, the leaching rate of rare earth is stable to more than 96%, two kinds of defective rare earth ores can be fully utilized, and the technical problem that the defective rare earth ore cannot be effectively and inexpensively treated in the prior art is solved;
2. the method has the advantages of stable product quality, good reproducibility, capacity of increasing the ore feeding amount of the rare earth concentrate by 8% in a single device, reduction of the unit consumption of the iron powder by more than 40%, and obvious economic benefit.
Drawings
FIG. 1 is a flowchart of the processing procedure of embodiment 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited to these examples.
Example 1
As shown in fig. 1, the method for treating a high-iron low-phosphorus rare earth ore provided in this embodiment specifically includes the following operations:
(1) Adding high-iron low-phosphorus rare earth ore into the rare earth concentrate, and uniformly mixing;
(2) Adding concentrated sulfuric acid into the mixed ore, uniformly mixing, placing the mixture into a high-temperature box type furnace, roasting at the low temperature of 280-300 ℃ for 60-120 min, then raising the temperature in the furnace to 400-420 ℃ until the fluid material is completely solidified, discharging, turning over a 200-mesh screen by using a small shovel, sieving, and adding magnesium sulfate water for leaching for 2h;
(3) Mixing slurry, performing filter pressing, neutralizing the filtrate, and performing filter pressing again to obtain a rare earth leachate; filter pressing the obtained filter residue after size mixing, carrying out slag washing and filter pressing, returning the filtrate obtained by slag washing to the size mixing procedure to be used as a liquid phase, and discharging the filter residue obtained by slag washing after soaking again; and returning filter residues obtained by neutralization to a size mixing procedure to be treated again as a solid phase.
The analysis results of the components of the rare earth concentrate and the high-iron low-phosphorus rare earth ore used in the present example are shown in table 1:
table 1 analysis results of ore raw material composition (%)
Analysis item REO PO 4 3- Fe 2 O 3 H2O F - CaO PbO
Baotou ore 59.43 17.39 2.90 8.75 6.26 8.76 <0.01
High-iron low-phosphorus rare earth ore 16.92 11.39 27.52 3.32 0.26 0.06 0.035
According to the method, the rare earth concentrate, the high-iron low-phosphorus rare earth ore and the iron powder are mixed according to different proportions, concentrated sulfuric acid with different ore-acid ratios is added, and the final result is shown in table 2.
Table 2 summary of the production results of different addition ratios
Baotou mineral (g) High-iron low-phosphorus rare earth ore (g) Iron powder addition g Mass ratio of mineral acid Decomposition Rate (%) Percent yield in REO (%)
100.00 0.00 15.25 1.5 95.9 96.41
95.00 5.00 12.50 1.5 95.92 97.18
90.00 10.00 8.75 1.5 95.27 96.66
85.00 15.00 6.75 1.5 94.91 96.40
80.00 20.00 0 1.5 94.55 96.24
75.00 25.00 0 1.5 96.38 95.05
70.00 30.00 0 1.5 94.01 93.12
90.00 10.00 8.75 1.7 96.25 96.62
85.00 15.00 6.75 1.7 96.01 96.76
80.00 20.00 0 1.7 95.03 96.53
As can be seen from Table 2, when the high-iron low-phosphorus rare earth ore accounts for 10-15% of the Baotou rare earth concentrate, the mineral acid ratio is 1.5, the leaching rate of the rare earth stably reaches more than 96%, the product quality is stable, the reproducibility is good, the ore feeding amount of the rare earth concentrate of a single device can be increased by 8%, the unit consumption of iron powder is reduced by more than 40%, and the economic benefit is obvious. After the optimal mixture ratio is selected, the production capacity and the cost reduction effect are continuously verified, the production capacity and the cost reduction are calculated according to the ore feeding amount of 50kg/min, and the results are shown in the table 3:
TABLE 3 productivity and cost reduction effects TABLE
Figure BDA0003792181150000041
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but any insubstantial modifications or changes made in the spirit and the spirit of the main design of the present invention, which still solves the technical problems consistent with the present invention, should be included in the scope of the present invention.

Claims (7)

1. The method for treating the high-iron low-phosphorus rare earth ore comprises a high-temperature reinforced roasting process of rare earth concentrate concentrated sulfuric acid, and is characterized in that before the concentrated sulfuric acid is added for roasting, high-iron low-phosphorus rare earth ore accounting for 10-15% of the total ore mass is also added into the rare earth concentrate, and rare earth occurrence structures of the high-iron low-phosphorus rare earth ore and the rare earth concentrate are phosphoric acid rare earth.
2. The method for treating the rare earth ore with high iron and low phosphorus content of claim 1, wherein the addition amount of the concentrated sulfuric acid is 1.5 to 1.7 times of the total mass of the rare earth ore with high iron and low phosphorus content and the rare earth concentrate.
3. A method of treating a high iron, low phosphorus rare earth ore according to claim 1 or 2, comprising the steps of:
(1) Adding high-iron low-phosphorus rare earth ore into the rare earth concentrate, and uniformly mixing;
(2) Adding concentrated sulfuric acid into the mixed ore, uniformly mixing, placing the mixture into a high-temperature box type furnace, roasting at the low temperature of 280-300 ℃ for 60-120 min, then raising the temperature in the furnace to 400-420 ℃ until the fluid material is completely solidified, discharging, turning and crushing by using a small shovel, returning the material to the high-temperature box type furnace, continuously roasting for 30-60 min, discharging, and turning and crushing by using the small shovel; returning the materials to the high-temperature box furnace again to continue roasting for 30-60 min, stopping the furnace, grinding the sample by using a sampling machine after the temperature is reduced, sieving the sample by using a sieve, and adding magnesium sulfate water to leach for 2h;
(3) And (3) size mixing, filter pressing, neutralizing the filtrate and carrying out filter pressing again to obtain the rare earth leaching solution.
4. The method for treating the rare earth ore with high iron and low phosphorus content according to claim 3, wherein in the step (1), iron powder accounting for 0-15% of the mass of the rare earth concentrate is added.
5. The method for treating a rare earth ore with high iron and low phosphorus content according to claim 3, wherein in the step (2), the screen is 200-mesh screen.
6. The method for treating the rare earth ore with high iron and low phosphorus according to claim 3, wherein in the step (3), the filter residue obtained by filter pressing after size mixing is subjected to slag washing and filter pressing, the filtrate obtained by slag washing is returned to the size mixing process to be used as a liquid phase, and the filter residue obtained by slag washing is discharged after being soaked again.
7. The method for treating the rare earth ore with high iron and low phosphorus content as claimed in claim 3, wherein in the step (3), the filter residue obtained by neutralization is returned to the size mixing process to be treated again as a solid phase.
CN202210959394.8A 2022-08-11 2022-08-11 Method for treating high-iron low-phosphorus rare earth ore Pending CN115449624A (en)

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Citations (10)

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Publication number Priority date Publication date Assignee Title
CN1721559A (en) * 2004-12-15 2006-01-18 北京有色金属研究总院 Process for comprehensive recovery of rare earth and thorium from rare earth ore
CN1847419A (en) * 2005-04-05 2006-10-18 内蒙古包钢稀土高科技股份有限公司 Stepped sulfuric acid treatment and roasting process for decomposing Baotou RE ore concentrate
CN101363079A (en) * 2007-08-10 2009-02-11 有研稀土新材料股份有限公司 Smelting method of iron rich mengite rare-earth mine
CN101633980A (en) * 2008-07-23 2010-01-27 甘肃稀土新材料股份有限公司 Roasting process of sulfuric acid of rare-earth ore
CN104561539A (en) * 2015-02-16 2015-04-29 包头市锦园化工科技有限公司 Energy-saving and high-efficiency rare earth ore concentrate sulfuric acid stepped roasting method
CN109097559A (en) * 2018-10-25 2018-12-28 西安西骏新材料有限公司 A kind of method that Bayan Obo rare earth ore concentrate produces mixed chlorinated rare earth
CN109988903A (en) * 2019-05-21 2019-07-09 李梅 A kind of method that concentrated sulfuric acid two-stage roasting decomposes high-grade mixed rare earth concentrates
CN111235382A (en) * 2020-02-18 2020-06-05 陕西德信祥能源科技有限公司 Environment-friendly and energy-saving rare earth concentrate sectional roasting system and roasting method
CN111363914A (en) * 2020-04-23 2020-07-03 西安三瑞实业有限公司 System and method for acidizing and roasting rare earth concentrate by using multi-section external heating rotary furnace
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CN1721559A (en) * 2004-12-15 2006-01-18 北京有色金属研究总院 Process for comprehensive recovery of rare earth and thorium from rare earth ore
CN1847419A (en) * 2005-04-05 2006-10-18 内蒙古包钢稀土高科技股份有限公司 Stepped sulfuric acid treatment and roasting process for decomposing Baotou RE ore concentrate
CN101363079A (en) * 2007-08-10 2009-02-11 有研稀土新材料股份有限公司 Smelting method of iron rich mengite rare-earth mine
CN101633980A (en) * 2008-07-23 2010-01-27 甘肃稀土新材料股份有限公司 Roasting process of sulfuric acid of rare-earth ore
CN104561539A (en) * 2015-02-16 2015-04-29 包头市锦园化工科技有限公司 Energy-saving and high-efficiency rare earth ore concentrate sulfuric acid stepped roasting method
CN109097559A (en) * 2018-10-25 2018-12-28 西安西骏新材料有限公司 A kind of method that Bayan Obo rare earth ore concentrate produces mixed chlorinated rare earth
CN109988903A (en) * 2019-05-21 2019-07-09 李梅 A kind of method that concentrated sulfuric acid two-stage roasting decomposes high-grade mixed rare earth concentrates
CN111235382A (en) * 2020-02-18 2020-06-05 陕西德信祥能源科技有限公司 Environment-friendly and energy-saving rare earth concentrate sectional roasting system and roasting method
CN111394571A (en) * 2020-04-17 2020-07-10 包头稀土研究院 Method for improving decomposition efficiency of rare earth mineral and sulfuric acid
CN111363914A (en) * 2020-04-23 2020-07-03 西安三瑞实业有限公司 System and method for acidizing and roasting rare earth concentrate by using multi-section external heating rotary furnace

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