CN117120643A - Method for recycling Sc from iron-aluminum slag in laterite-nickel ore high-pressure acid leaching process - Google Patents

Method for recycling Sc from iron-aluminum slag in laterite-nickel ore high-pressure acid leaching process Download PDF

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Publication number
CN117120643A
CN117120643A CN202380009965.4A CN202380009965A CN117120643A CN 117120643 A CN117120643 A CN 117120643A CN 202380009965 A CN202380009965 A CN 202380009965A CN 117120643 A CN117120643 A CN 117120643A
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iron
laterite
aluminum slag
recycling
nickel ore
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许开华
张文杰
张坤
彭亚光
金国泉
刘文泽
许鹏云
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Greenmei Indonesia New Energy Materials Co ltd
GEM Co Ltd China
Qingmeibang New Energy Materials Co ltd
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Greenmei Indonesia New Energy Materials Co ltd
GEM Co Ltd China
Qingmeibang New Energy Materials Co ltd
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    • 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 application discloses a method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process, which comprises the following steps: s1, leaching raw material iron aluminum slag by sulfuric acid, and performing filter pressing to obtain a leaching solution; s2, evaporating and concentrating the leaching solution to obtain a concentrated solution, and adding raw materials of iron aluminum slag and sodium sulfate into the concentrated solution to obtain a mixture; s3, carrying out pressurizing and heating treatment on the mixture, wherein the pressurizing pressure is 4.5-5.0MPa, the heating temperature is 250-260 ℃, and then carrying out solid-liquid separation to obtain a slag phase and a liquid phase; s4, sequentially extracting, back-extracting, precipitating scandium salt and roasting the liquid phase to obtain scandium oxide; high scandium recovery rate and simple steps.

Description

Method for recycling Sc from iron-aluminum slag in laterite-nickel ore high-pressure acid leaching process
Technical Field
The application relates to the technical field of metallurgy, in particular to a method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process.
Background
Sc is used as a rare-dispersion element and has important application in industry, but independent ore deposits are lacked, the content of Sc in primary ore deposits is extremely low, the recycling difficulty is high, and the cost is high, which is also the root cause of high price of Sc. The crude laterite-nickel ore generally contains 0.03-0.05% of Sc, and the content of impurities such as iron, aluminum, manganese, magnesium, calcium and the like in the laterite-nickel ore is high and far higher than that of scandium, so that scandium extraction is easy to be interfered, the direct extraction process is complicated, the impurity content is high, and the practical extraction significance is low.
In the related art, the patent with publication number CN 103468979 discloses a method for recovering scandium from laterite-nickel mining and smelting iron-aluminum slag, which comprises the steps of removing iron and aluminum by means of regulating pH, precipitating nickel and cobalt, obtaining sodium hydroxide scandium-nickel-cobalt precipitate, and recovering scandium from scandium-nickel-cobalt hydroxide precipitate.
In the method, because the impurity removal effect of each step is poor, various impurity removal modes are needed for impurity removal and enrichment, so that scandium loss is large, and raw materials and auxiliary materials are consumed more.
Disclosure of Invention
In view of the above, the application provides a method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process, which has the advantages of high scandium recovery rate and simple steps.
In order to achieve the technical purpose, the application adopts the following technical scheme:
the application provides a method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process, which comprises the following steps:
s1, leaching raw material iron aluminum slag by sulfuric acid, and performing filter pressing to obtain a leaching solution;
s2, evaporating and concentrating the leaching solution to obtain a concentrated solution, and adding raw materials of iron aluminum slag and sodium sulfate into the concentrated solution to obtain a mixture;
s3, carrying out pressurizing and heating treatment on the mixture, wherein the pressurizing pressure is 4.5-5.0MPa, the heating temperature is 250-260 ℃, and then carrying out solid-liquid separation to obtain a slag phase and a liquid phase;
s4, extracting, back extracting, precipitating scandium salt and roasting the liquid phase in sequence to obtain scandium oxide.
Preferably, in the step S4, the extracting agent used for extraction is a mixture of Cextran 230 extracting agent and N1923 extracting agent, the extracting agent uses sulfonated kerosene as a diluent, the mass ratio of the extracting agent Cextran 230 to N1923 is 1:1-4, the extracting agent is 20-50% in concentration, and the volume ratio of the extracting agent to the water phase is 2:1-3.
Preferably, in step S4, the stripping agent used for the stripping is EDTA solution.
Preferably, in step S4, the precipitant used for precipitating the scandium salt is an ammonium salt, the temperature of the precipitated scandium salt being 50-90 ℃.
Preferably, in step S4, the first organic phase obtained by extraction is washed with sulfuric acid between the extraction step and the back extraction step.
Preferably, in step S1, the pH value of the leaching treatment is 2-3, and the leaching time is 2-3h.
Preferably, the calcination temperature is 800-900 ℃.
Preferably, in step S2, the temperature of the evaporative concentration is 90-100 ℃.
Preferably, the slag phase comprises Fe 2 O 3 、Al 2 O 3 Sodium iron vitriol.
Preferably, after the stripping step, a scandium-containing stripping solution and a second organic phase are obtained, and the second organic phase is recycled and extracted continuously.
The beneficial effects of the application are as follows:
the application prepares high-purity scandium oxide by the process flow of normal pressure leaching-concentrating-high pressure impurity removal-extracting-back extraction-precipitation-roasting, has small loss rate of scandium (Sc) and short process flow, and is beneficial to scandium recovery;
according to the application, the pressurizing and heating treatment is utilized, so that iron ions and aluminum ions are hydrolyzed, meanwhile, the non-acid-leached iron aluminum slag is added in the reaction process, the hydrolysis reaction is promoted, meanwhile, sodium sulfate is also used for cooperatively removing the iron ions to form sodium-iron-vanadium, the hydrolysis reaction is further accelerated, the iron ions and aluminum ions are removed well, and the scandium recovery interference is reduced;
according to the application, the extraction agent system and the scandium precipitation system are adjusted to realize further improvement of scandium recovery.
Drawings
Fig. 1 is a process flow diagram of the present solution.
Detailed Description
The present application will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
As shown in FIG. 1, the application provides a method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process, which comprises the following steps:
s1, leaching raw material iron aluminum slag by sulfuric acid, and performing filter pressing to obtain a leaching solution;
s2, evaporating and concentrating the leaching solution to obtain a concentrated solution, and adding raw materials of iron aluminum slag and sodium sulfate into the concentrated solution to obtain a mixture;
s3, carrying out pressurizing and heating treatment on the mixture, wherein the pressurizing pressure is 4.5-5.0MPa, the heating temperature is 250-260 ℃, the reaction is carried out for 1-2h, and then solid-liquid separation is carried out to obtain a slag phase and a liquid phase;
s4, extracting, back extracting, precipitating scandium salt and roasting the liquid phase in sequence to obtain scandium oxide.
In the scheme, through the normal pressure sulfuric acid leaching of the step S1, the leaching rates of iron, aluminum and scandium can be basically leached, the concentration of Sc in the leaching liquid is low at the moment, and then through the concentration of the step S2, the concentration of Sc in the concentrated liquid is improved, and in the step S2, sodium sulfate is used for precipitating iron ions to form sodium jarosite, and the reaction mechanism is as follows: 3Fe 3+ +2SO 4 2- +Na + +6H 2 O→Na Fe 3 (SO 4 ) 2 (OH) 6 +6H + The method comprises the steps of carrying out a first treatment on the surface of the Under the condition of the step S3, the iron ions and the aluminum ions are hydrolyzed to form solid Fe 2 O 3 And Al 2 O 3 Entering slag items, releasing sulfuric acid, dissolving the generated sulfuric acid in the newly added raw material Fe-Al slag which is not leached under normal pressure in the step S2, promoting the chemical balance of hydrolysis reaction in the step S3 to go right, further precipitating iron and aluminum in the Fe-Al slag, further reducing Sc interference items in liquid phase, simultaneously, promoting the chemical balance of hydrolysis reaction to the right by sodium sulfate, and cooperatively removing Fe and Al with the raw material Fe-Al slag which is not leached under normal pressure in a high-pressure high-heat environment, thereby being beneficial to reducing the loss rate of Sc.
It is noted that, after the step of adding the raw materials of iron-aluminum slag and sodium sulfate into the concentrated solution in the step S2, in order to reduce the process flow, a solid-liquid mixture is directly obtained without performing solid-liquid separation treatment, and meanwhile, the solid-phase non-acid-leached raw materials of iron-aluminum slag can also be used as the raw materials of hydrolysis reaction in the step S3.
In the step S4, the extractant used for extraction is a mixture of Cextran 230 extractant and N1923 extractant, the extractant uses sulfonated kerosene as a diluent, the mass ratio of the extractant Cextran 230 to the N1923 is 1:1-4, the concentration of the extractant is 20-50%, and the volume ratio of the extractant to the water phase is 2:1-3.
In step S4, the stripping agent used for the stripping is EDTA solution.
In step S4, the precipitant used for precipitating scandium salt is ammonium salt, and the temperature of the scandium salt is 50-90 ℃.
In step S4, the first organic phase obtained by extraction is washed with sulfuric acid between the extraction step and the back extraction step.
In the step S1, the pH value of leaching treatment is 2-3, and the leaching time is 2-3h.
The roasting temperature is 800-900 ℃.
In step S2, the temperature of the evaporation concentration is 90-100 ℃.
The slag phase comprises Fe 2 O 3 、Al 2 O 3 Sodium iron vitriol.
And (3) after the back extraction step, obtaining scandium-containing back extraction liquid and a second organic phase, and recycling the second organic phase and continuing extraction.
Specifically, in step S4, the liquid phase obtained in step S3 is extracted by using a mixture of a cextran 230 extractant and an N1923 extractant to obtain a first organic phase and an extraction residual liquid, the first organic phase is washed by dilute sulfuric acid to obtain a first impurity-removed organic phase and a washing liquid containing impurities, the first impurity-removed organic phase is back-extracted by using an EDTA solution to obtain a second organic phase and a scandium-containing back-extracted liquid, the scandium-containing back-extracted liquid is precipitated by an ammonium salt and then baked to obtain scandium oxide, and the second organic phase is recycled to the extraction step for reuse.
The present application is further illustrated by the following specific examples.
Example 1
A method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process comprises the following steps:
s1, leaching raw material iron aluminum slag by sulfuric acid, wherein the pH value of the leaching treatment is 2, the leaching time is 3 hours, and leaching liquid is obtained after filter pressing;
s2, evaporating and concentrating the leaching solution, wherein the evaporating and concentrating temperature is 90 ℃, so as to obtain a concentrated solution, and adding raw materials of iron aluminum slag and sodium sulfate into the concentrated solution, so as to obtain a mixture;
s3, carrying out pressurizing and heating treatment on the mixture, wherein the pressurizing pressure is 4.5MPa, the heating temperature is 250 ℃, the reaction is carried out for 1-2h, and then solid-liquid separation is carried out to obtain a slag phase and a liquid phase;
s4, extracting the liquid phase obtained in the step S3 by using a mixture of a Cextran 230 extractant and an N1923 extractant, wherein the extractant uses sulfonated kerosene as a diluent, the mass ratio of the extractant Cextran 230 to the N1923 is 1:1, a first organic phase and an extraction residual liquid are obtained, the first organic phase is washed by dilute sulfuric acid, a first impurity-removing organic phase and a washing liquid containing impurities are obtained, the first impurity-removing organic phase is subjected to back extraction by using an EDTA solution, the volume ratio of the extractant to the water phase is 2:1, a second organic phase and a scandium-containing back extraction liquid are obtained, the scandium-containing back extraction liquid is subjected to precipitation at 90 ℃ by using ammonium sulfate, and then is roasted at 800 ℃, so that scandium oxide is obtained, and the second organic phase is reused in the extraction step.
Example 2
A method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process is the same as in example 1, except that in step S1, the leaching treatment is carried out at a pH value of 3 and a leaching time of 2 hours, in step S3, the pressurizing pressure is 5.0MPa, and the heating temperature is 260 ℃.
Comparative example 1
A method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process is the same as in example 1, except that in step S3, the pressurizing pressure is 1MPa, and the heating temperature is 200 ℃.
Comparative example 2
A method for recycling Sc from iron-aluminum slag in a high-pressure acid leaching process of laterite-nickel ores is the same as in example 1, except that sodium sulfate is not added in step S2.
Comparative example 3
A method for recycling Sc from iron-aluminum slag in a laterite-nickel ore high-pressure acid leaching process is the same as in example 1, except that no raw iron-aluminum slag is added in step S2.
Evaluation test
Scandium oxides obtained in examples 1 to 3 and comparative examples 1 to 3 were collected, and the scandium content in the primary iron-aluminum slag phase was determined by ICP, and the scandium recovery rate was calculated, and the results are shown in Table 1.
TABLE 1 scandium recovery rates for various schemes
Project Scandium recovery (%)
Example 1 81.52
Example 2 84.31
Example 3 80.36%
Comparative example 1 46.38
Comparative example 2 68.34
Comparative example 3 55.37
From the data, the scandium loss is small, and the recovery rate is high.
The present application is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present application are intended to be included in the scope of the present application.

Claims (10)

1. The method for recycling Sc from the iron-aluminum slag in the laterite-nickel ore high-pressure acid leaching process is characterized by comprising the following steps of:
s1, leaching raw material iron aluminum slag by sulfuric acid, and performing filter pressing to obtain a leaching solution;
s2, evaporating and concentrating the leaching solution to obtain a concentrated solution, and adding raw materials of iron aluminum slag and sodium sulfate into the concentrated solution to obtain a mixture;
s3, carrying out pressurizing and heating treatment on the mixture, wherein the pressurizing pressure is 4.5-5.0MPa, the heating temperature is 250-260 ℃, and then carrying out solid-liquid separation to obtain a slag phase and a liquid phase;
s4, extracting, back extracting, precipitating scandium salt and roasting the liquid phase in sequence to obtain scandium oxide.
2. The method for recycling Sc from iron-aluminum slag in the high pressure acid leaching process of laterite-nickel ore according to claim 1, wherein in the step S4, the extractant used in the extraction is a mixture of Cextran 230 extractant and N1923 extractant, the extractant uses sulfonated kerosene as a diluent, the mass ratio of the extractant Cextran 230 to N1923 is 1:1-4, the concentration of the extractant is 20-50%, and the volume ratio of the extractant to the water phase is 2:1-3.
3. The method for recycling Sc from iron-aluminum slag in high pressure acid leaching process of laterite-nickel ore as claimed in claim 1, wherein in step S4, the stripping agent used for stripping is EDTA solution.
4. The method for recycling Sc from iron-aluminum slag in high pressure acid leaching process of laterite-nickel ore according to claim 1, wherein in step S4, the precipitant used for precipitating scandium salt is ammonium salt, and the temperature of the precipitated scandium salt is 50-90 ℃.
5. The method for recycling Sc from iron-aluminum slag in high pressure acid leaching process of laterite-nickel ore according to claim 1, wherein in step S4, the first organic phase obtained by extraction is washed with sulfuric acid between the extraction step and the back extraction step.
6. The method for recycling Sc from iron-aluminum slag in a high pressure acid leaching process of laterite-nickel ore according to claim 1, wherein in step S1, the leaching treatment is carried out at a pH value of 2-3 for 2-3 hours.
7. The method for recovering Sc from laterite-nickel ore high pressure acid leaching process iron-aluminum slag according to claim 1, wherein the roasting temperature is 800-900 ℃.
8. The method for recycling Sc from iron-aluminum slag in high pressure acid leaching process of laterite-nickel ore as claimed in claim 1, wherein in step S2, the temperature of evaporation concentration is 90-100 ℃.
9. The method for recovering Sc from laterite-nickel ore high pressure acid leaching process iron-aluminum slag as set forth in claim 1, wherein the slag phase includes Fe 2 O 3 、Al 2 O 3 Sodium iron vitriol.
10. The method for recycling Sc from iron-aluminum slag in the high pressure acid leaching process of laterite-nickel ore according to claim 1, wherein after the back extraction step, a back extraction liquid containing scandium and a second organic phase are obtained, and the second organic phase is recycled and extracted continuously.
CN202380009965.4A 2023-06-30 2023-06-30 Method for recycling Sc from iron-aluminum slag in laterite-nickel ore high-pressure acid leaching process Pending CN117120643A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101768665A (en) * 2008-12-30 2010-07-07 厦门紫金矿冶技术有限公司 Method for reducing acid consumption during heap leaching and high-pressure leaching of nickel laterite ore
CN102312090A (en) * 2011-09-10 2012-01-11 吉林吉恩镍业股份有限公司 Process for extracting scandium from ore containing scandium through pressure leaching
CN103468979A (en) * 2013-08-15 2013-12-25 中国恩菲工程技术有限公司 Method for recycling scandium from lateritic nickel ore smelted iron aluminum slag
CN113392596A (en) * 2021-04-25 2021-09-14 四川大学 Method for extracting and separating scandium-iron solution by using microchannel reactor
CN114438348A (en) * 2021-12-29 2022-05-06 中南大学 Method for selectively extracting scandium from laterite-nickel ore
CN114737064A (en) * 2022-03-17 2022-07-12 云南云铜锌业股份有限公司 Zinc jarosite hydrometallurgy method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101768665A (en) * 2008-12-30 2010-07-07 厦门紫金矿冶技术有限公司 Method for reducing acid consumption during heap leaching and high-pressure leaching of nickel laterite ore
CN102312090A (en) * 2011-09-10 2012-01-11 吉林吉恩镍业股份有限公司 Process for extracting scandium from ore containing scandium through pressure leaching
CN103468979A (en) * 2013-08-15 2013-12-25 中国恩菲工程技术有限公司 Method for recycling scandium from lateritic nickel ore smelted iron aluminum slag
CN113392596A (en) * 2021-04-25 2021-09-14 四川大学 Method for extracting and separating scandium-iron solution by using microchannel reactor
CN114438348A (en) * 2021-12-29 2022-05-06 中南大学 Method for selectively extracting scandium from laterite-nickel ore
CN114737064A (en) * 2022-03-17 2022-07-12 云南云铜锌业股份有限公司 Zinc jarosite hydrometallurgy method

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