CN113104902A - A kind of method for preparing iron red from acid leaching slag of magnetic material waste - Google Patents
A kind of method for preparing iron red from acid leaching slag of magnetic material waste Download PDFInfo
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- CN113104902A CN113104902A CN202110373208.8A CN202110373208A CN113104902A CN 113104902 A CN113104902 A CN 113104902A CN 202110373208 A CN202110373208 A CN 202110373208A CN 113104902 A CN113104902 A CN 113104902A
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Abstract
The invention relates to the technical field of solid waste resource utilization, and discloses a method for preparing iron oxide red from magnetic material waste acid leaching slag, which comprises the following steps: (1) adding a hydrochloric acid solution into the magnetic material waste acid leaching residue, leaching, and filtering to obtain a leaching solution; (2) concentrating the leachate to obtain a concentrated ferric chloride solution; (3) adding water into the concentrated ferric chloride solution to dissolve the ferric chloride solution to obtain ferric chloride solution, and adding a reducing agent into the ferric chloride solution to convert ferric chloride into ferrous chloride; (4) adjusting the pH of the solution with a carbonate solution, removing impurities, and filtering to obtain a pure ferrous chloride solution; (5) and (3) dropwise adding a carbonate solution into the ferrous chloride solution obtained in the previous step to synthesize a ferrous carbonate precipitate. The method has the advantages of simple process and low production cost, and the produced iron oxide red has stable quality and meets the national high-class product standard.
Description
Technical Field
The invention relates to the technical field of solid waste resource utilization, in particular to a method for preparing iron oxide red from magnetic material waste acid leaching residues.
Background
The magnetic material waste acid leaching residue is waste residue generated after rare earth is extracted from neodymium iron boron waste by acid leaching, and the main component of the waste residue is Fe2O3And also contains a small amount of other metal elements. Because a small amount of hydrochloric acid is wrapped in the waste residues due to acid leaching, a large number of enterprises adopt landfill treatment or low-price sale as iron-making raw materials, which not only wastes secondary resources, but also has certain influence on the environment.
The traditional method for preparing the iron oxide red is to prepare the iron oxide red by using metallic iron, and with the increasing attention of people on the environment, vast scholars are dedicated to the research on the green production process for preparing the iron oxide red by using the iron-containing waste residues. Leaching the waste slag containing iron with sulfuric acid, purifying to obtain copperas, calcining copperas at high temperature to obtain iron oxide red, and discharging SO3And SO2The tail gas and tail gas treatment equipment is large in investment, and secondary pollution is caused to the environment if the tail gas and tail gas treatment equipment is not recycled. The wastewater generated by the ammonia process contains ammonium chloride or ammonium sulfate, and the wastewater discharge can be realized by recovering the ammonium chloride or the ammonium sulfate, but the process has the problem of incomplete seed crystal preparation, so that the quality of an iron oxide red product is unstable, and the application of the method is limited.
In addition, all methods for preparing iron oxide red by using seed crystals have the problem of difficult control in the link of oxidation by using air or oxygen, the problems of poor hue saturation and brightness of the iron oxide red can be caused by too fast or too slow ventilation, and the reaction time is long and can be generally finished within about 24 hours. The preparation method needs about 7 days for preparing the dark iron oxide red, the capacity is limited, the production input and output periods are long, and the recovery benefit is slow.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of harmful substances, high cost and unstable quality of the method for preparing iron oxide red in the prior art, thereby providing a method for preparing iron oxide red from acid leaching slag.
A method for preparing iron oxide red from magnetic material waste acid leaching slag comprises the following steps:
(1) adding a hydrochloric acid solution into the magnetic material waste acid leaching residue, leaching, and filtering to obtain a leaching solution;
(2) concentrating the leachate to obtain a concentrated ferric chloride solution;
(3) adding water into the concentrated ferric chloride solution to dissolve the ferric chloride solution to obtain ferric chloride solution, and adding a reducing agent into the ferric chloride solution to convert ferric chloride into ferrous chloride;
(4) adjusting the pH of the solution with a carbonate solution, removing impurities, and filtering to obtain a pure ferrous chloride solution; the carbonate solution is a sodium carbonate solution, a sodium bicarbonate solution, a potassium carbonate solution, a potassium bicarbonate solution or a magnesium carbonate solution;
(5) and (3) dropwise adding a carbonate solution into the ferrous chloride solution obtained in the previous step to synthesize a ferrous carbonate precipitate.
Optionally, the step (2) further comprises a step of recovering the hydrochloric acid solution.
Optionally, the concentration of the hydrochloric acid solution in the step (1) is 3-6 mol/L, and the ratio of the acid leaching waste residue to the hydrochloric acid is 1: (4-10), the ratio is g/mL;
optionally, the ratio of the acid leaching waste residue to the hydrochloric acid solution is 1: 6, the ratio is g/mL.
Optionally, the leaching temperature in the step (1) is 45-70 ℃, the time is 30-60 min, and the leaching times are 1-3;
optionally, the leaching temperature is 45-60 ℃ or 55-60 ℃, and the leaching time is 45-50 min.
Optionally, the concentration method in the step (2) is reduced pressure evaporation; the vacuum degree of the reduced pressure evaporation is 0.075MPa and-0.1 MPa, the evaporation temperature is 50-90 ℃, and the evaporation time is 30-90 minutes; optionally, the evaporation temperature is 70-75 ℃, and the evaporation time is 45-60 minutes.
Optionally, the reducing agent in the step (3) is iron sheet or scrap iron.
Optionally, the reduction reaction time in the step (3) is 12-36 hours, and the temperature is 70-95 ℃.
Optionally, in the step (3), the reduction reaction time is 24 hours, and the temperature is 80 ℃.
Optionally, the pH value in the step (4) is 3-5.
Optionally, the step (5) is followed by a step of filtering to obtain a ferrous carbonate precipitate, and drying and calcining the ferrous carbonate precipitate to obtain iron oxide red; the drying temperature is 85-105 ℃, and the calcining temperature is 700-780 ℃.
The technical scheme of the invention has the following advantages:
1. according to the method for preparing iron oxide red from the acid leaching residues, the acid leaching residues do not need to be further treated, so that the problem of environmental pollution caused by hydrochloric acid contained in the acid leaching residues is solved.
2. The method for preparing the iron oxide red from the acid leaching residues considers the problem of recycling hydrochloric acid after leaching iron elements by using excessive hydrochloric acid, and realizes the zero emission of pollutants at the stage.
3. According to the method for preparing the iron oxide red from the acid leaching residues, the adopted reducing agent iron sheet or iron scrap is waste which is obtained by using iron as a catalyst by a certain company, and secondary utilization of solid waste resources is realized again.
4. The method for preparing the iron oxide red from the acid leaching residues provided by the invention has the advantages of simple process and low production cost, and the produced iron oxide red has stable quality and meets the national high-class product standard.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of example 1.
Detailed Description
Example 1
The flow chart is shown in figure 1.
A method for preparing iron oxide red from magnetic material waste acid leaching slag comprises the following steps:
(1) taking 50.0g of magnetic material waste acid leaching residue, adding 300mL of 6.0mol/L hydrochloric acid solution, stirring for 30min at the temperature of 45 ℃, filtering and washing. And leaching the filter residue for 2 times according to the same conditions, wherein the dissolution rate of the obtained acid leaching waste residue is 83.8 percent, the total volume of the filtrate is 1000mL, and the total iron content in the filtrate is measured to be 24.5 g/L.
(2) Transferring the obtained filtrate into a rotary evaporator, adjusting the vacuum degree to 0.08MPa and the evaporation temperature to 70 ℃, and separating out orange crystals after evaporation for 30min, wherein the crystals are ferric trichloride crystals. And (4) continuing to evaporate until a small amount of liquid exists, stopping evaporation to obtain a concentrated ferric trichloride solution, wherein the concentration of the recovered hydrochloric acid solution is 3.9mol/L, and the recovered hydrochloric acid solution can be used for acid leaching and rare earth recovery.
(3) Adding water to the concentrated ferric trichloride solution to dissolve the concentrated ferric trichloride solution to 500mL, and mixing the solution according to a solid-to-liquid ratio of 1: 20 (the solid-liquid ratio is g/mL) is added with 25.0g of scrap iron, the temperature is kept for 24 hours at 80 ℃, and then the ferrous chloride solution is obtained by filtration. The filter residue is excessive scrap iron and can be repeatedly used.
(4) And (3) regulating the pH value of the ferrous chloride solution obtained in the last step to 5.0 by using a saturated sodium carbonate solution, generating flocculent precipitates which are aluminum precipitates and other impurities, and filtering to obtain a pure ferrous chloride solution. Saturated sodium carbonate solution is dripped into the pure ferrous chloride solution to synthesize ferrous carbonate precipitate, and the saturated sodium carbonate solution can be stopped dripping when the content of iron element in the solution is lower than 0.1 g/L.
(5) Filtering, washing the ferrous carbonate precipitate, drying in a drying oven at 105 ℃, then pouring into a magnetic crucible, and carrying out aerobic calcination at 700 ℃ for 30min to obtain 59.6g of iron oxide red.
Example 2
A method for preparing iron oxide red from magnetic material waste acid leaching slag comprises the following steps:
(1) taking 100.0g of magnetic material waste acid leaching waste residue, adding 600mL of 5.0mol/L hydrochloric acid solution, stirring for 45min at the temperature of 60 ℃, filtering and washing. And leaching the filter residue for 2 times according to the same conditions, wherein the dissolution rate of the obtained acid leaching waste residue is 83.9 percent, the total volume of the filtrate is 2000mL, and the total iron content in the filtrate is 24.6 g/L.
(2) Transferring the obtained filtrate into a rotary evaporator, adjusting the vacuum degree to 0.075MPa and the evaporation temperature to 75 ℃, and separating out orange crystals after evaporating for 45min, wherein the crystals are ferric trichloride crystals. And continuing to evaporate until a small amount of liquid exists, and stopping evaporation, wherein the concentration of the recovered hydrochloric acid solution is 4.1mol/L, and the recovered hydrochloric acid solution can be used for acid leaching and rare earth recovery.
(3) Adding water to the concentrated ferric trichloride solution to dissolve the concentrated ferric trichloride solution to 1000mL, and mixing the concentrated ferric trichloride solution with the solid-liquid ratio of 1: 20 (the solid-liquid ratio is g/mL) is added with 50.0g of scrap iron, the temperature is kept at 80 ℃ for 24 hours, and then the ferrous chloride solution is obtained by filtration. The filter residue is excessive scrap iron and can be repeatedly used.
(4) And (3) regulating the pH value of the ferrous chloride solution obtained in the last step to 4.5 by using a saturated sodium bicarbonate solution, generating flocculent precipitates, namely aluminum precipitates and other impurities, and filtering to obtain a pure ferrous chloride solution. Saturated sodium bicarbonate solution is dripped into the pure ferrous chloride solution to synthesize ferrous carbonate precipitate, and the dripping of the saturated sodium carbonate solution can be stopped when the content of iron element in the solution is lower than 0.1 g/L.
(5) Filtering, washing the ferrous carbonate precipitate, drying in a drying oven at 95 ℃, then pouring into a magnetic crucible, and carrying out aerobic calcination for 45min at 750 ℃ to obtain 118.5g of iron oxide red.
Example 3
A method for preparing iron oxide red from magnetic material waste acid leaching slag comprises the following steps:
(1) taking 200.0g of magnetic material waste acid leaching waste residue, adding 1200mL of 4.0mol/L hydrochloric acid, stirring for 50min at the temperature of 70 ℃, filtering and washing. And leaching the filter residue for 2 times according to the same conditions, wherein the dissolution rate of the obtained acid leaching waste residue is 83.6 percent, the total volume of the filtrate is 4000mL, and the total iron content in the filtrate is 24.3 g/L.
(2) Transferring the obtained filtrate into a rotary evaporator, adjusting the vacuum degree to 0.075MPa and the evaporation temperature to 75 ℃, and separating out orange crystals after evaporating for 60min, wherein the crystals are ferric trichloride crystals. And then continuing to evaporate until a small amount of liquid exists, and stopping evaporation, wherein the concentration of the recovered hydrochloric acid is 4.22mol/L, and the recovered hydrochloric acid can be used for acid leaching and rare earth recovery.
(3) Adding water to the concentrated ferric trichloride to dissolve the concentrated ferric trichloride to 2000mL, and mixing the iron trichloride and the water according to a solid-to-liquid ratio of 1: 20 (the solid-liquid ratio is g/mL) is added with 100.0g of scrap iron, the temperature is kept at 80 ℃ for 24 hours, and then the ferrous chloride solution is obtained by filtration. The filter residue is excessive scrap iron and can be repeatedly used.
(4) Using saturated MgCO to the ferrous chloride solution obtained in the last step3Adjusting the pH value of the solution to 4.0, generating flocculent precipitate which is aluminum and other impurities, and filtering to obtain a pure ferrous chloride solution. Adding saturated MgCO dropwise into pure ferrous chloride solution3Synthesizing ferrous carbonate precipitate with the solution, and stopping dripping saturated MgCO when the content of iron element in the solution is lower than 0.1g/L3And (3) solution.
(5) Filtering, washing the ferrous carbonate precipitate, drying in a drying oven at 85 ℃, then pouring into a magnetic crucible, and carrying out aerobic calcination at 780 ℃ for 50min to obtain 239.2g of iron oxide red.
Example 4
A method for preparing iron oxide red from magnetic material waste acid leaching slag comprises the following steps:
(1) taking 300.0g of magnetic material waste acid leaching waste residue, adding 1200mL of 6mol/L hydrochloric acid solution, stirring for 50min at the temperature of 50 ℃, filtering and washing. And leaching the filter residue for 2 times according to the same conditions, wherein the dissolution rate of the obtained acid leaching waste residue is 84.2 percent, the total volume of the filtrate is about 4000mL, and the total iron content in the filtrate is 24.7 g/L.
(2) Transferring the obtained filtrate into a rotary evaporator, adjusting the vacuum degree to 0.1MPa, the evaporation temperature to 90 ℃, and the evaporation time to 30min, and separating out orange crystals which are ferric trichloride crystals. And (4) continuing to evaporate until a small amount of liquid exists, stopping evaporation to obtain a concentrated ferric trichloride solution, wherein the concentration of the recovered hydrochloric acid solution is 3.9mol/L, and the recovered hydrochloric acid solution can be used for acid leaching and rare earth recovery.
(3) Dissolving concentrated ferric trichloride in water solution to 3000mL, and mixing the ferric trichloride solution with the solid-liquid ratio of 1: 20 (the solid-liquid ratio is g/mL), adding 150.0g of scrap iron, keeping the temperature at 70 ℃ for 36 hours, and then filtering to obtain a ferrous chloride solution. The filter residue is excessive scrap iron and can be repeatedly used.
(4) And (3) regulating the pH value of the ferrous chloride solution obtained in the last step to 5.0 by using a saturated potassium bicarbonate solution, generating flocculent precipitates, namely aluminum precipitates and other impurities, and filtering to obtain a pure ferrous chloride solution. Saturated potassium bicarbonate solution is dripped into the pure ferrous chloride solution to synthesize ferrous carbonate precipitate, and when the content of iron element in the solution is lower than 0.1g/L, the dripping of the saturated potassium bicarbonate solution can be stopped.
(5) Filtering, washing the ferrous carbonate precipitate, drying in a drying oven at 105 ℃, then pouring into a magnetic crucible, and carrying out aerobic calcination for 50min at 700 ℃ to obtain 356.2g of iron oxide red.
Example 5
A method for preparing iron oxide red from magnetic material waste acid leaching slag comprises the following steps:
(1) taking 500.0g of magnetic material waste acid leaching waste residue, adding 5000mL of 6mol/L hydrochloric acid solution, stirring for 60min at the temperature of 55 ℃, filtering and washing. The dissolution rate of the obtained acid leaching waste residue is 84.3 percent, the total volume is 5500mL, and the total iron content in the filtrate is measured to be 24.9 g/L.
(2) Transferring the obtained filtrate into a rotary evaporator, adjusting the vacuum degree to 0.076MPa and the evaporation temperature to 50 ℃, and separating out orange crystals after evaporation for 90min, wherein the crystals are ferric trichloride crystals. And then continuing to evaporate until a small amount of liquid exists, and stopping evaporation to obtain a concentrated ferric trichloride solution, wherein the concentration of the recovered hydrochloric acid solution is 4.08mol/L, and the recovered hydrochloric acid solution can be used for acid leaching and rare earth recovery.
(3) Adding water to the concentrated ferric trichloride solution to dissolve the concentrated ferric trichloride solution to 5000mL, and mixing the concentrated ferric trichloride solution with the solid-liquid ratio of 1: adding 250.0g of scrap iron into 20 (the solid-liquid ratio is g/mL), keeping the temperature at 95 ℃ for 12 hours, and then filtering to obtain a ferrous chloride solution. The filter residue is excessive scrap iron which can be reused.
(4) Using saturated K to the ferrous chloride solution obtained in the last step2CO3Adjusting the pH value of the solution to 5.0, generating flocculent precipitate which is aluminum precipitate and other impurities, and filtering to obtain pure ferrous chloride solution. Saturated K is dripped into pure ferrous chloride solution2CO3Solutions ofSynthesizing ferrous carbonate precipitate, and stopping dripping saturated K when the iron element content in the solution is lower than 0.1g/L2CO3And (3) solution.
(5) Filtering, washing the ferrous carbonate precipitate, drying in a drying oven at 105 ℃, then pouring into a magnetic crucible, and carrying out aerobic calcination for 60min at 750 ℃ to obtain 595.5g of iron oxide red.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
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| CN114314674A (en) * | 2021-12-24 | 2022-04-12 | 盐城工学院 | Preparation method of Fe oxide nano material applied to dechlorination of wastewater |
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