CN111549230A - Treatment method of neodymium iron boron waste - Google Patents

Treatment method of neodymium iron boron waste Download PDF

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CN111549230A
CN111549230A CN202010442980.6A CN202010442980A CN111549230A CN 111549230 A CN111549230 A CN 111549230A CN 202010442980 A CN202010442980 A CN 202010442980A CN 111549230 A CN111549230 A CN 111549230A
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iron boron
neodymium iron
boron waste
hydrochloric acid
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CN111549230B (en
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赵永志
马莹
帅国胜
候少春
笪宗扬
李二斗
丁艳蓉
张文娟
宋静
赵拓
王晶晶
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Baotou Rare Earth Research Institute
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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
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • 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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  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
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Abstract

The invention discloses a method for treating neodymium iron boron waste, which comprises the following steps: (1) mixing the neodymium iron boron waste with the solution A to obtain a mixture; adding hydrogen peroxide into the mixture, and reacting at 10-60 ℃ to obtain a first reactant; (2) adding the solution B into the first reactant for reaction to obtain a second reactant; wherein, the solution A is hydrochloric acid solution containing ammonium chloride; the solution B is one or more selected from hydrochloric acid solution, ammonium chloride aqueous solution and water. The invention can avoid high-temperature roasting and large amount of tail gas.

Description

Treatment method of neodymium iron boron waste
Technical Field
The invention relates to a method for treating neodymium iron boron waste, in particular to a method for treating neodymium iron boron waste at a low temperature.
Background
In recent years, with the development of the fields of wind power generation, new energy automobiles, medical instruments, aviation, war industry and the like, the demand of the neodymium iron boron magnetic material is gradually increased year by year. And a large amount of neodymium iron boron waste materials can be correspondingly generated due to the use of a large amount of neodymium iron boron magnets. In order to improve the secondary utilization rate of rare earth resources, the recovery of rare earth elements in neodymium iron boron waste materials is imperative.
In the recovery process of the neodymium iron boron waste, the pyrogenic process is relatively friendly to the environment, but the treatment capacity is small, the recovery rate is low, the energy consumption is high, and the recovery cost is high. The existing recovery process is mostly a wet process mainly comprising oxidizing roasting, acid dissolution and precipitation, the wet process has large treatment capacity, strong adaptability to neodymium iron boron waste materials and relatively low recovery cost, but the oxidizing roasting process has high energy consumption and large tail gas emission. Therefore, the development of the recovery process of the neodymium iron boron waste material, which has low energy consumption, no tail gas emission and good economic benefit, is an important research direction for the recovery of the neodymium iron boron waste material. In the recovery process of the neodymium iron boron waste, the oxidation of the neodymium iron boron waste is a very critical step.
CN103146925A discloses a method for recovering rare earth from neodymium iron boron waste, which comprises the steps of roasting, acidolysis, separation, firing and the like. CN106319249A discloses a method for recovering rare earth from neodymium iron boron waste. The neodymium iron boron waste is pretreated, then is roasted, is added with hydrochloric acid and hydrogen peroxide for acid leaching, and is neutralized. CN109554549A discloses a method for recovering rare earth in neodymium iron boron waste, which comprises the steps of oxidizing and roasting the neodymium iron boron waste; leaching the neodymium iron boron waste after oxidizing roasting with high-temperature high-pressure hydrochloric acid, then carrying out solid-liquid separation and collecting a liquid phase to obtain a leaching solution; adding an oxidant into the leachate to oxidize ferrous ions in the leachate into ferric ions; then, impurity removal and purification are carried out on the treated leachate, and then the leachate is filtered and the liquid phase is collected to obtain the rare earth chloride leachate. These methods employ a calcination process, which produces a large amount of off-gas.
In addition, the neodymium iron boron waste can be pretreated by a hydrochloric acid wetting-air oxidation method to oxidize iron elements into ferric iron (the natural oxidation pretreatment neodymium iron boron waste leaching process, dandeheng, nonferrous metal science and engineering, vol.8, No. 2, 2017). The hydrochloric acid used in the method has high concentration, and the volatilization of the hydrochloric acid causes pollution to the environment. In addition, the above method has low oxidation efficiency. After oxidizing for 20 days, the oxidation rate of the iron reaches 92.37 percent.
Disclosure of Invention
In view of this, the present invention aims to provide a method for treating neodymium iron boron waste, which can adopt low temperature oxidation, avoid high temperature roasting, and avoid emission of a large amount of tail gas. Further, the method can improve the oxidation efficiency of the neodymium iron boron waste. The invention adopts the following technical scheme to achieve the purpose.
The invention provides a method for treating neodymium iron boron waste, which comprises the following steps:
(1) mixing the neodymium iron boron waste with the solution A to obtain a mixture; adding hydrogen peroxide into the mixture, and reacting at 10-60 ℃ to obtain a first reactant;
(2) adding the solution B into the first reactant for reaction to obtain a second reactant;
wherein, the solution A is hydrochloric acid solution containing ammonium chloride; the solution B is one or more selected from hydrochloric acid solution, ammonium chloride aqueous solution and water.
According to the treatment method provided by the invention, the weight ratio of the solution A to the neodymium iron boron waste is preferably 0.1-0.35: 1.
According to the treatment method provided by the invention, the weight ratio of the solution A to the neodymium iron boron waste is preferably 0.15-0.35: 1.
According to the treatment method of the present invention, preferably, the concentration of hydrochloric acid in the solution A is 0.01 to 1.2mol/L, and the concentration of ammonium chloride in the solution A is 0.15 to 2.0 mol/L.
According to the treatment method, the weight ratio of the hydrogen peroxide to the neodymium iron boron waste is preferably 0.005-0.15; the concentration of the hydrogen peroxide is 15-30 wt%.
According to the treatment method provided by the invention, preferably, in the step (1), the reaction temperature is 20-50 ℃; the water content of the first reactant is less than or equal to 6 wt%.
According to the treatment method of the present invention, preferably, in the step (2), the solution B is water; or the solution B is a mixed solution consisting of a hydrochloric acid solution and an ammonium chloride aqueous solution, and in the mixed solution, the concentration of the hydrochloric acid is 0.001-0.15 mol/L, and the concentration of the ammonium chloride is 0.001-0.055 mol/L.
According to the treatment method provided by the invention, the weight ratio of the solution B to the neodymium iron boron waste is preferably 0.2-0.55: 1.
According to the treatment method of the present invention, preferably, in the step (2), the first reactant reacts with the solution B to form a reaction material; when the water content of the reaction material is less than or equal to 6 wt%, the supplementary solution B continues to react; circularly replenishing the solution B for a plurality of times and reacting until the oxidation rate of the iron is more than or equal to 95 percent; wherein the weight ratio of the solution B to the neodymium iron boron waste material supplemented each time is 0.2-0.55: 1.
According to the treatment method, the total reaction time of the step (1) and the step (2) is preferably 1-10 d.
According to the invention, the ammonium chloride-containing hydrochloric acid solution and the neodymium iron boron waste are reacted at a lower temperature, a small amount of hydrogen peroxide is used as a primer, and the solution B is supplemented in the reaction, so that the oxidation reaction is promoted, the oxidized neodymium iron boron waste with the iron oxidation rate of more than 95% is obtained, and the oxidation reaction time is only 1-10 days. The method of the invention avoids high-temperature roasting, thereby avoiding generating tail gas. Compared with the natural oxidation method, the method of the invention greatly improves the oxidation efficiency. Furthermore, the present invention can reduce the cost of oxidation.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the scope of the present invention is not limited thereto.
The method of the present invention includes a step of generating a first reactant and a step of generating a second reactant. Which are separately described below.
< step of producing first reactant >
Mixing the neodymium iron boron waste material with the solution A to obtain a mixture. The mixing manner is not particularly limited as long as the neodymium iron boron waste can be uniformly mixed with the solution a. When mixing, solution a is preferably added to the neodymium iron boron scrap. The particle size of the neodymium iron boron waste material is 100-200 meshes, preferably 100-180 meshes, and more preferably 120-160 meshes. Solution a is a hydrochloric acid solution containing ammonium chloride.
The weight ratio of the solution A to the neodymium iron boron waste is 0.1-0.35: 1, preferably 0.15-0.35: 1, and more preferably 0.15-0.3: 1. Thus being beneficial to realizing the oxidation reaction of the solution A and the neodymium iron boron waste at lower temperature and improving the oxidation efficiency. The invention unexpectedly discovers that the efficiency of the oxidation reaction of the neodymium iron boron waste can be greatly improved by adding ammonium chloride into the hydrochloric acid solution.
In the solution A, the concentration of hydrochloric acid is 0.01-1.2 mol/L, and the concentration of ammonium chloride is 0.15-2.0 mol/L. Preferably, the concentration of the hydrochloric acid in the solution A is 0.01-1.1 mol/L, and the concentration of the ammonium chloride in the solution A is 0.15-1.8 mol/L. More preferably, the concentration of hydrochloric acid in the solution A is 0.02-1.0 mol/L, and the concentration of ammonium chloride is 0.18-1.8 mol/L. Thus being beneficial to improving the oxidation efficiency and reducing the oxidation cost.
According to one embodiment of the invention, neodymium iron boron waste is mixed with solution A to obtain a mixture; the mesh number of the neodymium iron boron waste is 100-160 meshes, the solution A is a hydrochloric acid solution containing ammonium chloride, and the weight ratio of the solution A to the neodymium iron boron waste is 0.15-0.35: 1.
According to a preferred embodiment of the present invention, neodymium iron boron waste is mixed with solution a to obtain a mixture; wherein the mesh number of the neodymium iron boron waste is 120-160 meshes, the solution A is a hydrochloric acid solution containing ammonium chloride, and the weight ratio of the solution A to the neodymium iron boron waste is 0.15-0.3: 1.
In the present invention, the hydrochloric acid solution containing ammonium chloride is a mixed solution of hydrochloric acid and ammonium chloride. In certain embodiments, the ammonium chloride-containing hydrochloric acid solution is formulated from concentrated hydrochloric acid, ammonium chloride solids, and water. In other embodiments, the ammonium chloride-containing hydrochloric acid solution is formulated from concentrated hydrochloric acid, ammonium chloride-containing wastewater produced during the rare earth smelting process, and water. In still other embodiments, the ammonium chloride-containing hydrochloric acid solution is formulated from concentrated hydrochloric acid and the ammonium chloride solids and water produced after evaporative crystallization of the ammonium chloride wastewater. In still other embodiments, the hydrochloric acid solution containing ammonium chloride is prepared from concentrated hydrochloric acid, ammonium chloride solids, and condensed water generated during evaporative crystallization of ammonium chloride wastewater. Preferably, the hydrochloric acid solution containing ammonium chloride is prepared from concentrated hydrochloric acid, waste water containing ammonium chloride generated in the rare earth smelting process and water. This further reduces the cost of oxidation and allows for waste recycling.
Adding hydrogen peroxide into the mixture, and reacting at 10-60 ℃ to obtain a first reactant. The above reaction may be carried out under the condition of contacting with air. Thus, the oxidation reaction can be carried out by utilizing the oxygen in the air, thereby saving the cost. Mixing the neodymium iron boron waste with the solution A to obtain a mixture, standing for 0-10 min, and adding a hydrogen peroxide oxidant into the mixture. The invention discovers that hydrogen peroxide can be used as a primer to promote the oxidation reaction of the neodymium iron boron waste. The reason for this is probably that the inert substances on the surface of the neodymium iron boron waste material can be removed by using hydrochloric acid in the solution a, and then hydrogen peroxide, ammonium chloride and hydrochloric acid are added to synergistically promote oxidation.
The concentration of the hydrogen peroxide is 15-30 wt%, preferably 20-30 wt%, and more preferably 25-30 wt%. The weight ratio of the hydrogen peroxide to the neodymium iron boron waste is 0.005-0.15: 1, preferably 0.01-0.15: 1, and more preferably 0.01-0.1: 1. This makes it possible, on the one hand, to increase the oxidation efficiency and, on the other hand, to reduce the costs. The invention discovers that when the dosage of the hydrogen peroxide is too small, the hydrogen peroxide cannot synergistically act with the ammonium chloride and the hydrochloric acid to promote the oxidation; if the dosage of the hydrogen peroxide is too much, the influence on the oxidation efficiency is not great, the cost is increased, and the synergistic effect of the hydrogen peroxide, the ammonium chloride and the hydrochloric acid is not facilitated. Therefore, the weight ratio of the hydrogen peroxide to the neodymium iron boron waste is controlled to be 0.005-0.15: 1.
The mixture reacts in the presence of hydrogen peroxide to obtain a first reactant. The reaction temperature is 10-60 ℃, preferably 15-55 ℃, and more preferably 20-50 ℃. This facilitates the oxidation reaction and avoids high temperature calcination.
In the present invention, the water content of the first reactant is controlled to 6 wt% or less, preferably 5 wt% or less, and more preferably 3 wt% or less. This is advantageous for improving the oxidation efficiency.
According to one embodiment of the invention, 30 wt% of hydrogen peroxide is added into the mixture and reacts at 20-55 ℃ to obtain a first reactant; wherein the weight ratio of the hydrogen peroxide to the neodymium iron boron waste is 0.01-0.1: 1.
According to another embodiment of the invention, 30 wt% of hydrogen peroxide is added into the mixture and reacts at 20-50 ℃ to obtain a first reactant; wherein the weight ratio of the hydrogen peroxide to the neodymium iron boron waste is 0.01-0.15: 1.
According to another embodiment of the invention, 30 wt% of hydrogen peroxide is added into the mixture and reacts at 20-40 ℃ to obtain a first reactant; wherein the weight ratio of the hydrogen peroxide to the neodymium iron boron waste is 0.01-0.1: 1.
< step of producing second reactant >
Adding the solution B into the first reactant for reaction to obtain a second reactant. The solution B is one or more selected from hydrochloric acid solution, ammonium chloride aqueous solution and water. In certain embodiments, solution B is water. In other embodiments, solution B is a mixed solution consisting of a hydrochloric acid solution and an aqueous ammonium chloride solution. More preferably, the solution B is a mixed solution composed of a hydrochloric acid solution and an aqueous ammonium chloride solution.
In a preferred embodiment, the solution B is a mixed solution consisting of a hydrochloric acid solution and an ammonium chloride aqueous solution, and the concentration of the hydrochloric acid in the mixed solution is 0.001-0.15 mol/L, and the concentration of the ammonium chloride in the mixed solution is 0.001-0.055 mol/L. Preferably, the concentration of the hydrochloric acid is 0.001-0.13 mol/L, and the concentration of the ammonium chloride is 0.001-0.05 mol/L. More preferably, the concentration of hydrochloric acid is 0.001-0.1 mol/L, and the concentration of ammonium chloride is 0.001-0.04 mol/L.
In certain embodiments, solution B is formulated from a hydrochloric acid solution and an aqueous ammonium chloride solution. In other embodiments, solution B is prepared from concentrated hydrochloric acid, ammonium chloride wastewater produced during the rare earth smelting process, and condensed water produced during the ammonium chloride wastewater treatment process.
The weight ratio of the solution B to the neodymium iron boron waste is 0.2-0.55: 1, preferably 0.2-0.5: 1, and more preferably 0.25-0.5: 1. This is advantageous for improving the oxidation efficiency.
In certain embodiments, a reaction mass is formed during the reaction of the first reactant with solution B; when the water content of the reaction material is less than or equal to 6 wt%, the supplementary solution B continues to react; the replenishing solution B is circulated for a plurality of times and reacts until the oxidation rate of the iron is more than or equal to 95 percent. Wherein the weight ratio of the solution B to the neodymium iron boron waste material supplemented each time is 0.2-0.55: 1.
In other embodiments, a reaction mass is formed during the reaction of the first reactant with solution B; when the water content of the reaction material is less than or equal to 3 wt%, the supplementary solution B continues to react; the replenishing solution B is circulated for a plurality of times and reacts until the oxidation rate of the iron is more than or equal to 95 percent. The weight ratio of the solution B to the neodymium iron boron waste material supplemented each time is 0.2-0.5: 1.
In still other embodiments, a reaction mass is formed during the reaction of the first reactant with solution B; when the water content of the reaction material is less than or equal to 3 wt%, the supplementary solution B continues to react; the replenishing solution B is circulated for a plurality of times and reacts until the oxidation rate of the iron is more than or equal to 95 percent. The weight ratio of the solution B to the neodymium iron boron waste material supplemented each time is 0.25-0.5: 1.
In the present invention, the number of times of replenishing the solution B is generally six or more. The water used in the invention is preferably deionized water, and more preferably condensed water obtained by evaporating and concentrating ammonium chloride wastewater generated in the rare earth smelting process.
In the invention, when the oxidation rate of iron is more than or equal to 95%, a second reactant is obtained, and the second reactant is the oxidized neodymium iron boron waste. And (3) the oxidation rate of the iron in the second reactant is greater than or equal to 95%, and the oxidized neodymium iron boron waste material with the oxidation rate of the iron greater than or equal to 95% is obtained. The obtained oxidized neodymium iron boron waste can be used for the next treatment. The total reaction time of the step (1) and the step (2) is 1-10 d, preferably 2-7 d, and more preferably 3-6 d. The reaction time of the leaching process of the neodymium iron boron waste material pretreated by natural oxidation in the prior art is more than 20 days. By adopting the treatment method, the oxidation efficiency is greatly improved.
The invention can obtain the oxidized neodymium iron boron waste, but avoids high-temperature roasting and generation of a large amount of tail gas. Compared with the method for pretreating the neodymium iron boron waste material by natural oxidation in the leaching process in the prior art, the method has the advantage that the oxidation efficiency is greatly improved. But also can recycle the ammonium chloride waste water.
< measuring method >
In the invention, the oxidation rate of iron is measured by a potassium dichromate titration method.
In the present invention, the water content is measured by a gravimetric method.
The starting materials used in the following examples and comparative examples are illustrated below:
the particle size of the neodymium iron boron waste is 120-160 meshes.
The hydrogen peroxide is 30 wt%.
The solution A and the solution B are prepared from concentrated hydrochloric acid, ammonium chloride wastewater generated in the rare earth smelting process and condensed water generated in the ammonium chloride wastewater treatment process.
Example 1
Uniformly mixing 100g of neodymium iron boron waste material and 25g of solution A (the concentration of hydrochloric acid is 0.5mol/L, and the concentration of ammonium chloride is 1.2mol/L) to obtain a mixture; adding 1g of hydrogen peroxide into the mixture, and reacting at 30 ℃ to obtain a first reactant. The water content of the first reactant was 3 wt%.
Adding 25g of solution B (the concentration of hydrochloric acid is 0.02mol/L, the concentration of ammonium chloride is 0.01mol/L) into the first reactant to continue the reaction, and forming a reaction material; when the water content in the reaction materials is 2 wt%, 25g of solution B is supplemented for continuous reaction; the circularly supplemented solution B reacts until the oxidation rate of the iron is more than or equal to 95 percent, and a second reactant is obtained.
Example 2
Uniformly mixing 100g of neodymium iron boron waste material and 25g of solution A (the concentration of hydrochloric acid is 0.8mol/L, and the concentration of ammonium chloride is 1.0mol/L) to obtain a mixture; adding 3g of hydrogen peroxide into the mixture, and reacting at 40 ℃ to obtain a first reactant. The water content of the first reactant was 3 wt%.
Adding 25g of solution B (the concentration of hydrochloric acid is 0.01mol/L, the concentration of ammonium chloride is 0.02mol/L) into the first reactant to continue the reaction, and forming a reaction material; when the water content in the reaction materials is 2 wt%, 25g of solution B is supplemented for continuous reaction; the circularly supplemented solution B reacts until the oxidation rate of the iron is more than or equal to 95 percent, and a second reactant is obtained.
Example 3
Uniformly mixing 1500g of neodymium iron boron waste material and 250g of solution A (the concentration of hydrochloric acid is 0.9mol/L, and the concentration of ammonium chloride is 1.2mol/L) to obtain a mixture; adding 50g of hydrogen peroxide into the mixture, and reacting at 35 ℃ to obtain a first reactant. The water content of the first reactant was 2 wt%.
Adding 500g of solution B (the concentration of hydrochloric acid is 0.03mol/L, the concentration of ammonium chloride is 0.01mol/L) into the first reactant to continue the reaction, and forming a reaction material; when the water content in the reaction materials is 2 wt%, 500g of solution B is supplemented for continuous reaction; the circularly supplemented solution B reacts until the oxidation rate of the iron is more than or equal to 95 percent, and a second reactant is obtained.
Comparative example 1
The only difference from example 1 is that the amount of hydrogen peroxide was 20 g.
Comparative example 2
The only difference from example 1 is that solution a is a hydrochloric acid solution, containing no ammonium chloride; the solution B is water.
TABLE 1
Numbering Time of oxidation reaction/d Oxidation rate of iron/%)
Example 1 6 96.8
Example 2 3 95.6
Example 3 5 96.5
Comparative example 1 5 96.9
Comparative example 2 35 95.2
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.

Claims (10)

1. The treatment method of the neodymium iron boron waste is characterized by comprising the following steps:
(1) mixing the neodymium iron boron waste with the solution A to obtain a mixture; adding hydrogen peroxide into the mixture, and reacting at 10-60 ℃ to obtain a first reactant;
(2) adding the solution B into the first reactant for reaction to obtain a second reactant;
wherein, the solution A is hydrochloric acid solution containing ammonium chloride; the solution B is one or more selected from hydrochloric acid solution, ammonium chloride aqueous solution and water.
2. The treatment method according to claim 1, wherein the weight ratio of the solution A to the neodymium iron boron waste is 0.1-0.35: 1.
3. The treatment method according to claim 2, wherein the weight ratio of the solution A to the neodymium iron boron waste is 0.15-0.35: 1.
4. The method according to claim 1, wherein the hydrochloric acid concentration in the solution A is 0.01 to 1.2mol/L, and the ammonium chloride concentration is 0.15 to 2.0 mol/L.
5. The treatment method according to claim 1, wherein the weight ratio of the hydrogen peroxide to the neodymium iron boron waste is 0.005-0.15; the concentration of the hydrogen peroxide is 15-30 wt%.
6. The processing method according to claim 1,
in the step (1), the reaction temperature is 20-50 ℃; the water content of the first reactant is less than or equal to 6 wt%.
7. The processing method according to claim 1,
in the step (2), the solution B is water; or the solution B is a mixed solution consisting of a hydrochloric acid solution and an ammonium chloride aqueous solution, and in the mixed solution, the concentration of the hydrochloric acid is 0.001-0.15 mol/L, and the concentration of the ammonium chloride is 0.001-0.055 mol/L.
8. The treatment method according to any one of claims 1 to 7, wherein in the step (2), the weight ratio of the solution B to the neodymium iron boron waste is 0.2-0.55: 1.
9. The process of claim 8, wherein in step (2), the first reactant reacts with solution B to form a reaction mass; when the water content of the reaction material is less than or equal to 6 wt%, the supplementary solution B continues to react; circularly replenishing the solution B for a plurality of times and reacting until the oxidation rate of the iron is more than or equal to 95 percent; wherein the weight ratio of the solution B to the neodymium iron boron waste material supplemented each time is 0.2-0.55: 1.
10. The process of claim 9, wherein the total reaction time of step (1) and step (2) is 1-10 days.
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CN108018429A (en) * 2017-12-28 2018-05-11 长春工程学院 A kind of method that room temperature ultrasound-hydrogen peroxide wet oxidation removes the impurity such as iron removaling and organic matter from neodymium iron boron waste material

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CN103146925A (en) * 2013-03-25 2013-06-12 安徽天泽矿业科技发展有限公司 Method of recycling rear earth from neodymium iron boron waste
CN103540756A (en) * 2013-10-29 2014-01-29 中南大学 Method for dissolving out rare-earth by treating waste neodymium-iron-boron materials
CN103773966A (en) * 2014-03-03 2014-05-07 绵竹华垒化工有限责任公司 Method for separating and utilizing neodymium iron boron waste materials
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CN108018429A (en) * 2017-12-28 2018-05-11 长春工程学院 A kind of method that room temperature ultrasound-hydrogen peroxide wet oxidation removes the impurity such as iron removaling and organic matter from neodymium iron boron waste material

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