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WO2025000487A1 - Procédé d'élimination de fer et d'aluminium d'un lixiviat de minerai de nickel latéritique au moyen d'un procédé goethite - Google Patents

Procédé d'élimination de fer et d'aluminium d'un lixiviat de minerai de nickel latéritique au moyen d'un procédé goethite Download PDF

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Publication number
WO2025000487A1
WO2025000487A1 PCT/CN2023/105016 CN2023105016W WO2025000487A1 WO 2025000487 A1 WO2025000487 A1 WO 2025000487A1 CN 2023105016 W CN2023105016 W CN 2023105016W WO 2025000487 A1 WO2025000487 A1 WO 2025000487A1
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WO
WIPO (PCT)
Prior art keywords
iron
aluminum
stage
nickel ore
removal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/CN2023/105016
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English (en)
Chinese (zh)
Inventor
许开华
刘维
张坤
彭亚光
金国泉
刘文泽
许鹏云
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pt Gem Indonesia New Energy Materials
Pt Qmb New Energy Materials
GEM Co Ltd Korea
Original Assignee
Pt Gem Indonesia New Energy Materials
Pt Qmb New Energy Materials
GEM Co Ltd Korea
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pt Gem Indonesia New Energy Materials, Pt Qmb New Energy Materials, GEM Co Ltd Korea filed Critical Pt Gem Indonesia New Energy Materials
Priority to PCT/CN2023/105016 priority Critical patent/WO2025000487A1/fr
Priority to CN202380009964.XA priority patent/CN117098860A/zh
Publication of WO2025000487A1 publication Critical patent/WO2025000487A1/fr
Anticipated expiration legal-status Critical
Pending legal-status Critical Current

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Classifications

    • 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
    • C22B23/00—Obtaining nickel or cobalt
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes

Definitions

  • the invention belongs to the field of solution purification in hydrometallurgy, and in particular relates to a method for removing iron and aluminum from laterite nickel ore leaching solution by a goethite method.
  • pressure leaching technology Since its introduction, pressure leaching technology has been industrially applied in the extraction of metals such as zinc, copper, manganese, and aluminum.
  • the use of pressure acid leaching to treat laterite nickel ore has the advantages of high nickel and cobalt leaching rates and effective separation of iron, aluminum, and nickel and cobalt.
  • MHP nickel-cobalt
  • the main methods used to remove iron in China are iron hydroxide method, yellow sodium iron alum method, and goethite method.
  • the yellow sodium iron alum method has strict requirements on the temperature of iron removal, a long alum formation time, and a relatively large amount of yellow sodium iron alum slag, and has certain requirements on the concentration of alkali metal ions in the solution;
  • the iron hydroxide method generates Fe(OH) 3 colloidal precipitation, which is difficult to filter and contains a high content of nickel, cobalt and manganese metals in the slag, resulting in a certain waste of resources.
  • the precipitation method is one of the important wet iron removal methods, and the goethite method is one of the effective iron removal methods.
  • the ferrous ions in the solution are first oxidized, then the temperature is adjusted to 80-100°C, and then a precipitant is added to adjust the pH value to 4.0-6.0, allowing the iron ions to precipitate in the form of goethite.
  • the traditional goethite method only adjusts the pH and temperature during the iron and aluminum removal process, and the pH and temperature used are both high, which may generate iron hydroxide colloids. This type of slag is difficult to filter and will absorb a large amount of nickel, cobalt and manganese, resulting in serious waste of metals such as nickel, cobalt and manganese while removing iron and aluminum impurities.
  • the present invention aims to provide a method for removing laterite by goethite.
  • the method for removing iron and aluminum from nickel ore leaching solution combines the goethite method with the neutralization hydrolysis method and is carried out in two stages.
  • By reasonably controlling parameters such as pH and feed rate efficient removal of iron and aluminum impurities is achieved at a lower nickel, cobalt and manganese consumption.
  • the iron removal by goethite method usually requires strict control of the pH of the system.
  • a high pH value is prone to produce iron hydroxide colloids, resulting in high nickel loss; if the pH is too low, iron cannot be completely removed.
  • the inventors of the present application realized that in addition to pH, the feed rate also has a significant impact on the iron and aluminum content in the impurity removal liquid.
  • a too fast feed rate will lead to an excessively high iron concentration to generate iron hydroxide colloids, and the nickel precipitation loss rate will also increase. Therefore, the present invention was created considering the influence of the feed rate.
  • the present invention provides a method for removing iron and aluminum from laterite nickel ore leaching solution by a goethite method, comprising the following steps:
  • One-stage iron and aluminum removal add precipitant solution to the laterite nickel ore leaching solution, control the feed rate to 5-80mL/min, pH to 3.0-3.2, reaction temperature to 60-70°C, react for 45-90min, and obtain a first-stage iron and aluminum slag and filtrate after solid-liquid separation;
  • Second stage iron and aluminum removal add precipitant solution to the filtrate, control the pH to 4.3-4.4, the reaction temperature to 60-70°C, react for 30-60 minutes, separate the solid and liquid, and obtain second stage iron and aluminum slag and purified liquid.
  • the laterite nickel ore leaching solution may contain a small amount of Fe 2+ .
  • an oxidant is added to the leaching solution to oxidize Fe 2+ into Fe 3+ .
  • the oxidant is sodium chlorate or air.
  • the oxidant is air
  • a sufficient amount of catalyst Cu 2+ needs to be added.
  • the laterite nickel ore leachate is pre-neutralized to a pH of 1.5 to 2.5, and then CCD washing is performed. Pre-neutralization reduces the acid content to obtain a qualified solution for goethite precipitation.
  • the pre-neutralized solution produces a supernatant and slag after CCD washing, and the supernatant is used for goethite precipitation, which reduces the amount of neutralizer used during precipitation and avoids excessive content of nickel, cobalt, etc. in the iron precipitation slag.
  • the pH value of the one-stage iron and aluminum removal of the present invention is relatively low.
  • the one-stage iron and aluminum slag is added to the pre-neutralization liquid to adjust the pH value of the one-stage iron and aluminum removal system, thereby reducing the consumption of the precipitant.
  • the pH value used in the second-stage iron and aluminum removal is relatively high.
  • the second-stage iron and aluminum slag is added to the leachate to pre-neutralize and adjust the pH value of the leachate, which not only reduces the consumption of the precipitant, but also dissolves the nickel and cobalt contained in the residue back into the leachate, thereby improving the separation efficiency of nickel and cobalt.
  • the precipitant solution is limestone slurry with a mass concentration of 20%.
  • the feed rate is 10-50 mL/min
  • the reaction temperature is 70° C.
  • the pH is 3.1
  • the reaction time is 60-90 min.
  • the feed rate is 10 mL/min and the reaction time is 90 min.
  • the reaction temperature is 60° C. and the reaction time is 60 min.
  • the goethite method of the present invention removes iron and aluminum, adopts a continuous feeding method, and is carried out in two stages.
  • the first stage controls the feeding speed to 5-80mL/min, the pH is 3.0-3.2, the reaction temperature is 60-70°C, and the reaction time is 45-90min, so that the iron element is retained in the filter residue as much as possible to improve the iron removal rate;
  • the second stage is unidirectionally fed with a precipitant solution to adjust the pH value to 4.3-4.4, the reaction temperature is 60-70°C, and the reaction time is 30-60min, and the aluminum ions and the remaining iron ions are precipitated.
  • the present invention realizes the effective separation of iron and aluminum in the leachate at a relatively low pH and temperature by controlling the feeding speed, the overall iron and aluminum removal efficiency is high, the slag particles produced are large, the filtering performance is good, and the valuable metals such as nickel, cobalt and manganese entrained in the slag are small, the iron and aluminum content in the slag is high, and the overall process flow is simple.
  • the present invention adds the first-stage iron-aluminum slag to the pre-neutralization solution to adjust the pH value of the first-stage iron-aluminum removal system, thereby reducing the consumption of the precipitant; by adding the second-stage iron-aluminum slag to the leaching solution to adjust the pH value of the leaching solution, not only the consumption of the precipitant is reduced, but also the nickel and cobalt contained in the residue are reversely dissolved into the leaching solution, thereby improving the separation efficiency of nickel and cobalt.
  • Fig. 1 is a process flow chart of the present invention
  • FIG2 is a curve diagram of the iron and aluminum content and nickel precipitation rate in the first stage of iron and aluminum removal filtrate at different feed rates
  • FIG3 is a curve diagram of the iron and aluminum content and nickel precipitation rate in a first stage of iron and aluminum removal filtrate at different pH values
  • FIG4 is a curve diagram of the iron and aluminum content and the nickel precipitation rate in a first stage of iron and aluminum removal filtrate under different time conditions
  • FIG5 is a curve diagram of the iron and aluminum content in the purified liquid of the second-stage iron and aluminum removal under different pH and time conditions
  • FIG. 6 is a graph showing the aluminum content in the purified liquid of the second-stage iron and aluminum removal under different temperature conditions.
  • the method for removing iron and aluminum from laterite nickel ore leachate by a goethite method comprises the following steps:
  • Second stage iron and aluminum removal Continue to add precipitant solution to the reactor, control the pH of the solution in the reactor to 4.3, the temperature to 60°C, react for 60 minutes, and obtain second stage iron and aluminum slag and purified liquid after filtration.
  • the first-stage iron filter residue in step (3) is recycled into the pre-neutralization solution to adjust the pH value of the first-stage iron-aluminum removal system; and the second-stage iron-aluminum residue in step (4) is added into the acid leaching solution for pre-neutralization.
  • Example 2 The same process as in Example 1 was used to remove iron and aluminum, except that the feed rates in the first stage of iron and aluminum removal were 10 mL/min, 20 mL/min, 30 mL/min, 40 mL/min, 50 mL/min, 60 mL/min, 70 mL/min, and 80 mL/min, respectively.
  • the iron and aluminum contents and the nickel precipitation rates in the filtrates of the first stage of iron and aluminum removal in Examples 1 to 9 are shown in Table 1 and Figure 2.
  • the present invention achieves a high iron removal rate while retaining the nickel content in the filtrate by controlling the feed rate; in Example 2, when the feed rate is controlled to be 10 mL/min, the pH is 3.1, the temperature is 70°C, and the stabilization time is 60 min, it has the highest iron and aluminum removal effect, and the nickel loss rate is low.
  • the iron and aluminum removal was carried out in the same process as in Example 1, except that the pH in the first stage of iron and aluminum removal was controlled to be 3.0 and 3.2 respectively.
  • the iron and aluminum removal was carried out according to the same process as in Example 2, except that the stabilization time in the iron and aluminum removal was controlled to be 45 minutes and 90 minutes respectively.
  • the iron and aluminum removal was carried out according to the same process as in Example 1, except that the reaction time in the second stage of iron and aluminum removal was controlled to be 30 minutes.
  • the iron and aluminum removal was carried out in the same process as in Example 1, except that the pH of the system was controlled to be 4.4 in the second-stage iron and aluminum removal.
  • the iron and aluminum removal was carried out in the same process as in Example 1, except that the reaction temperature in the second stage of iron and aluminum removal was controlled to be 70°C.
  • the iron and aluminum removal was carried out according to the same process as in Example 1, except that the pH of the system was controlled to be 2.7, 2.9, 3.3, 3.5, 3.7, and 3.9 in the first stage of iron and aluminum removal.
  • the iron and aluminum content and the nickel precipitation rate in the filtrate of the first stage of iron and aluminum removal under different pH conditions are shown in Table 2 and Figure 3.
  • the iron and aluminum were removed according to the same process as in Example 2, except that the stabilization time in the first stage of iron and aluminum removal was controlled to be 15 min and 30 min respectively.
  • the iron and aluminum contents and the nickel precipitation rate in the filtrate of the first stage of iron and aluminum removal under different time conditions are shown in Table 3 and Figure 4.
  • the present invention controls the stabilization time to be 45-90min to achieve a high iron removal rate while avoiding a large amount of nickel loss, wherein the stabilization time is preferably 60-90min, and 90min is the best. Since the present invention also includes recycling a section of iron-aluminum slag for dissolution of nickel in the pre-neutralization solution, the stabilization time is selected to be 60min in the actual production process.
  • the iron and aluminum removal was carried out according to the same process as in Example 1, except that the pH of the control system in the second stage iron and aluminum removal was 4.1, 4.5, 4.7, and 4.9, respectively, and the reaction time was 30 min and 60 min, respectively.
  • the iron and aluminum contents in the purified liquid of the second stage iron and aluminum removal under different pH and time conditions are shown in Table 4 and Figure 5.
  • the aluminum was removed by the same process as in Example 1, except that the temperature of the control system in the second stage of aluminum removal was 40° C. and 50° C., respectively. Since the iron element was basically completely removed in the first stage of impurity removal, this comparative example only tested the aluminum content in the second stage of aluminum removal purification liquid under different temperature conditions as shown in Table 5 and Figure 6.
  • the concentration of aluminum generally decreases first and then increases.
  • the aluminum removal rate is highest when the temperature is 60-70°C. Therefore, the temperature of the second-stage iron and aluminum removal of the present invention is preferably 60-70°C, more preferably 60°C.
  • the present invention adopts a two-stage iron and aluminum removal process using a goethite method, which improves the iron and aluminum removal efficiency while also taking into account the precipitation rate of nickel and cobalt.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

L'invention concerne un procédé d'élimination du fer et de l'aluminium d'un lixiviat de minerai de nickel latéritique au moyen d'un procédé goethite, lequel procédé comprend les étapes suivantes : l'élimination de fer et d'aluminium de première étape, consistant à : ajouter une solution de précipitant à un lixiviat de minerai de nickel latéritique, faire réagir celui-ci pendant 45 à 90 minutes avec la vitesse d'alimentation régulée à environ 5 à 80 mL/min, le pH étant régulé à environ 3,0 à 3,2 et la température de réaction étant régulée à environ 60 à 70 °C, et effectuer une séparation solide-liquide, de façon à obtenir des résidus de fer et d'aluminium de première étape et un filtrat ; et l'élimination de fer et d'aluminium de deuxième étape, consistant à : ajouter une solution de précipitant au filtrat, faire réagir celui-ci pendant 30 à 60 minutes avec le pH régulé à environ 4,3 à 4,4 et la température de réaction régulée à environ 60 à 70 °C, et effectuer une séparation solide-liquide, de façon à obtenir des résidus de fer et d'aluminium de deuxième étape et un liquide purifié. Une élimination de fer et d'aluminium en deux étapes est utilisée ; dans la première étape, des ions fer dans le lixiviat sont efficacement séparés à une valeur de pH relativement faible par régulation de la vitesse d'alimentation, des particules de résidu générées sont importantes, une bonne performance de filtration est obtenue et peu de métaux de valeur tels que le nickel, le cobalt et le manganèse sont entraînés dans les résidus ; dans la deuxième étape, le pH est régulé à environ 4,3 à 4,4 pour précipiter des ions aluminium et les ions fer restants ; et tout le processus technologique est simple.
PCT/CN2023/105016 2023-06-30 2023-06-30 Procédé d'élimination de fer et d'aluminium d'un lixiviat de minerai de nickel latéritique au moyen d'un procédé goethite Pending WO2025000487A1 (fr)

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PCT/CN2023/105016 WO2025000487A1 (fr) 2023-06-30 2023-06-30 Procédé d'élimination de fer et d'aluminium d'un lixiviat de minerai de nickel latéritique au moyen d'un procédé goethite
CN202380009964.XA CN117098860A (zh) 2023-06-30 2023-06-30 一种针铁矿法去除红土镍矿浸出液中铁和铝的方法

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CN120404364A (zh) * 2025-07-03 2025-08-01 高速铁路建造技术国家工程研究中心 一种红黏土中游离氧化铁去除效果定量评价方法及系统

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CN120404364A (zh) * 2025-07-03 2025-08-01 高速铁路建造技术国家工程研究中心 一种红黏土中游离氧化铁去除效果定量评价方法及系统
CN120404364B (zh) * 2025-07-03 2025-09-16 高速铁路建造技术国家工程研究中心 一种红黏土中游离氧化铁去除效果定量评价方法及系统

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