CN113667824A - Method for separating rare earth and iron from neodymium iron boron waste material with high selectivity - Google Patents
Method for separating rare earth and iron from neodymium iron boron waste material with high selectivity Download PDFInfo
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- CN113667824A CN113667824A CN202110800313.5A CN202110800313A CN113667824A CN 113667824 A CN113667824 A CN 113667824A CN 202110800313 A CN202110800313 A CN 202110800313A CN 113667824 A CN113667824 A CN 113667824A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention relates to the field of comprehensive recycling of rare earth solid waste resources, in particular to a method for separating rare earth and iron from neodymium iron boron waste with high selectivity; in the invention, the neodymium iron boron waste is oxidized and roasted, so that metal elements in the neodymium iron boron waste are converted into oxides; uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, directly roasting to convert rare earth in the neodymium iron boron waste into rare earth oxide which is easy to dissolve in dilute acid, converting iron element into fayalite which is not easy to dissolve in dilute acid, and then leaching with dilute acid to realize high-efficiency separation of rare earth and iron; the obtained rare earth leachate can be directly used for an extraction separation production line to recover rare earth, and the obtained fayalite can be used as a refractory material; the method has the characteristics of simple process, low cost, less pollution, high selectivity and capability of synthesizing rare earth and iron.
Description
Technical Field
The invention relates to the field of comprehensive recycling of rare earth solid waste resources, in particular to a method for separating rare earth and iron from neodymium iron boron waste with high selectivity.
Background
The neodymium iron boron waste contains 27% -32% of rare earth and 67% -73% of iron, the rare earth is a national strategic resource, the rare earth in the neodymium iron boron waste can be recycled, the rare earth mining can be reduced, the environmental pollution is reduced, and the sustainable development of the rare earth magnetic material is realized.
The industrial recovery of Nd-Fe-B waste material is usually carried out by wet method, mainly including hydrochloric acid optimum dissolution method, hydrochloric acid full dissolution method, complex salt precipitation method, etc., wherein the hydrochloric acid optimum dissolution method is to oxidize and calcine Nd-Fe-B waste material under proper condition, and add industrial concentrated hydrochloric acid (volume fraction)>31%) to make rare earth be preferentially dissolved out, then regulating pH value to make partial dissolved iron be precipitated, and feeding the obtained rare earth leachate into extraction separation production line. The hydrochloric acid full-dissolving method is to dissolve all rare earth and iron in the neodymium iron boron waste into hydrochloric acid, and then add oxidant to make Fe2+Conversion to Fe3+And adjusting the pH value to precipitate iron to obtain the rare earth leaching solution. The double salt precipitation is to dissolve iron and rare earth in the neodymium iron boron waste into sulfuric acid, add sodium sulfate to convert the rare earth into rare earth sodium double salt precipitation, and the ferric sulfate/ferrous iron is left in the liquid phase, thereby realizing the separation of the rare earth and iron.
In conclusion, during the acid leaching of neodymium iron boron, rare earth is leached out while a large amount of or all iron is leached out, an iron precipitation process is required to be added subsequently, the consumption of acid and an iron precipitation agent is high, iron resources are not recycled, and secondary harm is caused to the environment due to storage, so that a high-selectivity leaching separation process is developed, and the method has important significance for comprehensively recovering neodymium iron boron waste.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a method for separating rare earth and iron from neodymium iron boron waste materials with high selectivity, which oxidizes and roasts the neodymium iron boron waste materials to convert metal elements in the neodymium iron boron waste materials into oxides; uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, directly roasting to convert rare earth in the neodymium iron boron waste into rare earth oxide which is easy to dissolve in dilute acid, converting iron element into fayalite which is not easy to dissolve in dilute acid, and then leaching with dilute acid to realize high-efficiency separation of rare earth and iron; the obtained rare earth leachate can be directly used for an extraction separation production line to recover rare earth, and the obtained fayalite can be used as a refractory material.
The technical scheme for solving the technical problem is as follows:
a method for separating rare earth and iron from neodymium iron boron waste material with high selectivity comprises the following steps:
step S1, oxidizing and roasting the neodymium iron boron waste;
step S2, uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, and roasting to obtain neodymium iron boron roasted sand;
and step S3, uniformly mixing the neodymium iron boron calcine and the leaching agent, and filtering to obtain the rare earth leaching liquid and the fayalite.
As an improvement of the invention, in step S1, the neodymium iron boron waste is oxidized and roasted for 30-120 min at the temperature of 300-500 ℃.
As a further improvement of the invention, the silicon additive is silica.
As a further improvement of the invention, the reducing agent is at least one of Fe, C and Si.
In a further improvement of the present invention, in step S2, the oxidized neodymium iron boron waste is mixed with a silicon additive according to a molar ratio of iron to silicon of 1.8 to 2.1.
As a further improvement of the invention, in step S2, the amount of the reducing agent is Fe in the neodymium iron boron waste2O3The molar weight of all the converted FeO is 0.8-1.2 times.
As a further improvement of the invention, in step S3, the neodymium iron boron calcine and the leaching agent are mixed, stirred for 60-180 min at 40-80 ℃, and filtered to obtain the rare earth leaching liquid and the fayalite.
As a further improvement of the present invention, in step S3, the leaching agent is at least one of diluted hydrochloric acid, diluted nitric acid, diluted sulfuric acid and diluted acetic acid.
As a further improvement of the invention, the concentration of the leaching agent is 0.5-3 mol/L.
As a further improvement of the invention, in step S3, the solid-to-liquid ratio of the leaching solution is (3-10): 1.
in the invention, the neodymium iron boron waste is oxidized and roasted, so that metal elements in the neodymium iron boron waste are converted into oxides; uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, directly roasting to convert rare earth in the neodymium iron boron waste into rare earth oxide which is easy to dissolve in dilute acid, converting iron element into fayalite which is not easy to dissolve in dilute acid, and then leaching with dilute acid to realize high-efficiency separation of rare earth and iron; the obtained rare earth leachate can be directly used for an extraction separation production line to recover rare earth, and the obtained fayalite can be used as a refractory material; the method has the characteristics of simple process, low cost, less pollution, high selectivity and capability of synthesizing rare earth and iron.
Drawings
For ease of illustration, the present invention is described in detail by the following preferred embodiments and the accompanying drawings.
FIG. 1 is a block diagram of the steps of the present invention;
FIG. 2 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1 and fig. 2, the method for separating rare earth and iron from neodymium iron boron waste with high selectivity of the invention comprises the following steps:
step S1, oxidizing and roasting the neodymium iron boron waste;
step S2, uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, and roasting to obtain neodymium iron boron roasted sand;
and step S3, uniformly mixing the neodymium iron boron calcine and the leaching agent, and filtering to obtain the rare earth leaching liquid and the fayalite.
In the invention, the neodymium iron boron waste is oxidized and roasted, so that metal elements in the neodymium iron boron waste are converted into oxides; uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, directly roasting to convert rare earth in the neodymium iron boron waste into rare earth oxide which is easy to dissolve in dilute acid, converting iron element into fayalite which is not easy to dissolve in dilute acid, and then leaching with dilute acid to realize high-efficiency separation of rare earth and iron; the obtained rare earth leachate can be directly used for an extraction separation production line to recover rare earth, and the obtained fayalite can be used as a refractory material; the method has the characteristics of simple process, low cost, less pollution, high selectivity and capability of synthesizing rare earth and iron.
In the invention, in step S1, the neodymium iron boron waste is oxidized and roasted for 30min to 120min at the temperature of 300 ℃ to 500 ℃, so that metal elements in the neodymium iron boron waste are converted into oxides.
In step S2, mixing the oxidized neodymium iron boron waste with a silicon additive according to the molar ratio of iron to silicon of 1.8-2.1, wherein the amount of the reducing agent is Fe in the neodymium iron boron waste2O3The molar weight of all the silicon-containing compounds converted into FeO is 0.8-1.2 times, wherein the silicon additive adopts silicon dioxide, and the reducing agent is at least one of Fe, C and Si; uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, and then roasting, wherein the roasting atmosphere is an inert atmosphere, the roasting temperature is 700-1300 ℃, and the roasting time is 60-240 min.
In the invention, in step S3, mixing the neodymium iron boron calcine with a leaching agent, stirring for 60-180 min at 40-80 ℃, and filtering to obtain a rare earth leaching solution and fayalite, wherein the leaching agent is at least one of dilute hydrochloric acid, dilute nitric acid, dilute sulfuric acid and dilute acetic acid, and the concentration of the leaching agent is 0.5-3 mol/L; the solid-to-solid ratio of the leaching solution is (3-10): 1.
in the invention, after the neodymium iron boron waste is oxidized and roasted, metal elements in the neodymium iron boron waste are converted into oxides, and iron oxides in the oxidized waste are converted into fayalite in the roasting process of a silicon additive and a reducing agent, and the related reaction equation is as follows:
| 4Nd+3O2=2Nd2O3 | (1) |
| 4Fe+3O2====Fe2O3 | (2) |
| 2Fe2O3+3SiO2+2Fe==== 3Fe2SiO4 | (3) |
| 2Fe2O3+SiO2+Si==== 2Fe2SiO4 | (4) |
| 2Fe2O3+SiO2+C==== 2Fe2SiO4+CO2 | (5) |
specifically, after being roasted by silicon dioxide and a reducing agent, main phases existing in the neodymium iron boron roasted sand are rare earth oxide and fayalite, wherein the rare earth oxide is easy to dissolve out in a dilute acid, and the fayalite is difficult to dissolve out in the dilute acid, so that the high-selectivity separation of the rare earth and iron is realized.
The rare earth leachate obtained by the method has low iron content, does not need an iron precipitation process, can be directly used for a rare earth extraction production line, simplifies the process, reduces the reagent consumption, and the obtained fayalite has low acidity and high purity, can be used for manufacturing refractory materials, and realizes comprehensive recycling of resources.
The method has the advantages of simple process, low cost and pollution reduction, and can realize the low-acid high-selectivity leaching of the rare earth, and the obtained fayalite can be comprehensively recycled.
For better illustration, the invention provides several examples, as follows:
example one
Taking 6.88 g of neodymium iron boron waste (the Fe content is 44 wt%), the granularity is less than 30 μm, carrying out oxidizing roasting for 120min at 300 ℃ in a muffle furnace, adding 2.56 g of silicon dioxide and 1.48 g of iron powder into the oxidized waste, uniformly mixing the two materials, preparing a cylindrical block with the diameter of 30mm under the pressure of 20Mpa, putting the cylindrical block into a corundum crucible, putting the corundum crucible into an atmosphere furnace for roasting, heating the atmosphere furnace temperature to 1100 ℃ at 10 ℃/min, keeping the temperature for 2 hours, cooling the materials to room temperature along with the furnace after the heat preservation is finished, taking out the materials for grinding, putting the ground materials into a beaker, adding 2mol/L HCl 70ml, heating in a water bath to 80 ℃, stirring for 2 hours at 200rpm, and filtering and separating to obtain rare earth leachate and fayalite, wherein the rare earth leaching rate is 95.81%, and the Fe leaching rate is 2.34%.
Example two
Taking 6.88 g of neodymium iron boron waste (the Fe content is 44 wt%), the granularity is less than 30 μm, carrying out oxidizing roasting for 120min at 300 ℃ in a muffle furnace, adding 0.83 g of silicon dioxide and 0.41 g of silicon powder into the oxidized waste, uniformly mixing the two materials, preparing a columnar block with the diameter of 30mm under the pressure of 30Mpa, putting the columnar block into a corundum crucible, putting the corundum crucible into an atmosphere furnace for roasting, heating the atmosphere furnace temperature to 1000 ℃ at 10 ℃/min, keeping the temperature for 3 hours, cooling the materials to room temperature along with the furnace after the heat preservation is finished, taking out the materials for grinding, putting the ground materials into a beaker, adding 60ml of 1.2 mol/L HCl, heating in a water bath to 80 ℃, stirring for 2 hours at 200rpm, and filtering and separating to obtain rare earth leachate and fayalite, wherein the leaching rate of the rare earth is 96.65%, and the leaching rate of Fe is 1.26%.
EXAMPLE III
6.88 g of neodymium iron boron waste (the content of Fe is 44 wt.%) is taken, and the granularity is<30 μm, oxidizing and roasting at 300 deg.C in muffle furnace for 120min, adding 1.71 g of silicon dioxide and 0.18 g of carbon powder into the oxidized waste, mixing the two materials, and adding corundumPlacing the corundum crucible in a crucible, roasting in an atmosphere furnace, heating the temperature of the atmosphere furnace from room temperature to 1000 ℃ at a speed of 10 ℃/min, preserving heat for 4 hours, cooling the materials to room temperature along with the furnace after the heat preservation is finished, taking out the materials, grinding, placing the ground materials into a beaker, and adding 3mol/L H2SO450ml, heated to 50 ℃ in water bath, stirred for 2 hours at 200rpm, filtered and separated to obtain rare earth leachate and fayalite, and the results are obtained, wherein the leaching rate of the rare earth is 94.82 percent, and the leaching rate of the Fe is 0.89 percent.
The results of examples one to three are compared as follows:
 |
example one | Example two | EXAMPLE III |
| Leaching rate of rare earth | 95.81% | 96.65% | 94.82% |
| Iron leaching rate | 2.34% | 1.26% | 0.89% |
In the first to third embodiments, the leaching rate of rare earth is over 94%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A method for separating rare earth and iron from neodymium iron boron waste material with high selectivity is characterized by comprising the following steps:
step S1, oxidizing and roasting the neodymium iron boron waste;
step S2, uniformly mixing the oxidized neodymium iron boron waste with a silicon additive and a reducing agent, and roasting to obtain neodymium iron boron roasted sand;
and step S3, uniformly mixing the neodymium iron boron calcine and the leaching agent, and filtering to obtain the rare earth leaching liquid and the fayalite.
2. The method for separating the rare earth and the iron from the neodymium iron boron waste with high selectivity according to claim 1, wherein in step S1, the neodymium iron boron waste is subjected to oxidizing roasting at 300-500 ℃ for 30-120 min.
3. The method for separating the rare earth and the iron in the neodymium iron boron waste material with high selectivity according to claim 1, wherein the silicon additive is silicon dioxide.
4. The method for separating the rare earth and the iron in the neodymium iron boron waste material with high selectivity according to claim 1, wherein the reducing agent is at least one of Fe, C and Si.
5. The method for separating the rare earth and the iron in the neodymium iron boron waste material with high selectivity according to claim 3, wherein in step S2, the oxidized neodymium iron boron waste material is mixed with the silicon additive according to the molar ratio of the iron to the silicon being 1.8-2.1.
6.The method for separating the rare earth and the iron in the ndfeb waste with high selectivity according to claim 4, wherein in step S2, the amount of the reducing agent is Fe in the ndfeb waste2O3The molar weight of all the converted FeO is 0.8-1.2 times.
7. The method for separating rare earth and iron from neodymium iron boron waste with high selectivity as claimed in claim 1, wherein in step S3, neodymium iron boron calcine and leaching agent are mixed, stirred for 60 min-180 min at 40-80 ℃, and filtered to obtain rare earth leachate and fayalite.
8. The method for separating rare earth and iron from neodymium iron boron waste with high selectivity according to claim 7, wherein in step S3, the leaching agent is at least one of diluted hydrochloric acid, diluted nitric acid, diluted sulfuric acid and diluted acetic acid.
9. The method for separating rare earth and iron from neodymium iron boron waste with high selectivity according to claim 8, wherein the concentration of the leaching agent is 0.5-3 mol/L.
10. The method for separating the rare earth and the iron in the neodymium iron boron waste material with high selectivity according to claim 9, wherein in step S3, the ratio of leaching solution to solid is (3-10): 1.
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Cited By (1)
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| CN116377521A (en) * | 2022-12-30 | 2023-07-04 | 中国科学院江西稀土研究院 | Method for recycling mixed rare earth from NdFeB waste |
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| CN116377521A (en) * | 2022-12-30 | 2023-07-04 | 中国科学院江西稀土研究院 | Method for recycling mixed rare earth from NdFeB waste |
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