KR101664827B1 - Method for recovering nickel and cobalt - Google Patents
Method for recovering nickel and cobalt Download PDFInfo
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- KR101664827B1 KR101664827B1 KR1020150122496A KR20150122496A KR101664827B1 KR 101664827 B1 KR101664827 B1 KR 101664827B1 KR 1020150122496 A KR1020150122496 A KR 1020150122496A KR 20150122496 A KR20150122496 A KR 20150122496A KR 101664827 B1 KR101664827 B1 KR 101664827B1
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- cobalt
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- raw material
- reducing
- acid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/005—Preliminary treatment of ores, e.g. by roasting or by the Krupp-Renn process
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
-
- 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
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- 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
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0438—Nitric acids or salts thereof
-
- 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
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0446—Leaching processes with an ammoniacal liquor or with a hydroxide of an alkali or alkaline-earth metal
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
- C22B23/0469—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods by chemical substitution, e.g. by cementation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
Abstract
The method of recovering nickel and cobalt according to the present invention comprises the steps of adding a raw material containing nickel cobalt and a coal powder to a reducing furnace to obtain a reducing raw material, And recovering nickel and cobalt from the raw material having a low content of nickel and cobalt while reducing the recovery of iron and recovering the nickel and cobalt at a high recovery rate There is an effect to recover.
Description
The present invention relates to a process for recovering nickel and cobalt from low-grade raw materials having a low content of nickel and cobalt.
Due to the depletion of high-grade ore containing nickel, a process for extracting nickel and cobalt from raw materials having a low nickel content has been developed and commercialized or under development. In the case of a raw material having a low nickel content, for example, in the case of low-quality light, a relatively large amount of raw materials and energy are consumed due to a low nickel content, so that it is difficult to extract nickel and cobalt by conventional techniques.
In order to overcome such manufacturing disadvantages, a process for extracting only nickel and cobalt from low-level light at high temperature and high pressure (hereinafter, HPAL process, High Pressure Acid Leaching) has been developed. In addition, a process of recovering nickel and cobalt through ammonia leaching after the reduction process and recovering ammonia again (hereinafter, Caron process) was developed and commercialized.
Examples of techniques for recovery of nickel by the HPAL method include Korean Patent Laid-Open Publication No. 2007-7020915 and Japanese Laid-Open Patent Publication No. 2010-031341. Since the HPAL method should be carried out under high temperature and high pressure, continuous operation is difficult, and a large amount of expensive high-temperature and high-pressure reactors must be used. Also, it is known that it is mainly used for the titanium material because of its strong acidity, and accordingly, the equipment cost is very high and the maintenance cost is high. Furthermore, since it is necessary to use caustic soda as an expensive precipitating agent for concentrating nickel or to use an environmentally hazardous precipitating agent such as H 2 S, there is a problem in that equipment cost for treating such an agent is increased.
In the Caron process, it is possible to operate the process at a lower pressure than the HPAL because it can be operated at atmospheric pressure. However, the recovery rate of nickel and cobalt is usually as low as 80% and 50%, respectively.
The present invention proposes a method for effectively recovering nickel and cobalt from a low-quality raw material having a low content of nickel and cobalt.
According to an embodiment of the present invention, there is provided a process for producing a reducing raw material, comprising the steps of: introducing a mixed raw material containing nickel cobalt-containing raw material and coal powder into a reducing furnace to obtain a reducing raw material; slurrying the reducing raw material in an inert atmosphere to prepare a slurry; And introducing the leaching agent into the slurry to obtain leachate containing nickel and cobalt.
And drying the nickel cobalt-containing raw material.
The drying may be performed at a temperature ranging from 40 to 250 ° C.
The nickel cobalt-containing raw material may be limonite, saponite, or a mixture thereof.
The coal powder may be at least one selected from the group consisting of bituminous coal, semi-anthracite coal and anthracite coal.
The weight ratio of the nickel-cobalt-containing raw material and the coal powder may be 100: 0.1 to 50.
The reducing furnace may have a temperature of 250 to 800 ° C.
The slurry includes the reducing raw material and water, and the weight ratio of the reducing raw material and water may be 1: 1 to 25.
The precipitant may be at least one selected from the group consisting of sulfuric acid, a sulfate, hydrochloric acid, hydrochloric acid, nitric acid, nitric acid salt, hydrofluoric acid, hydrofluoric acid, phosphoric acid, phosphate, acetic acid, acetic acid salt, propionic acid, propionic acid salt, ammonium salt, aluminum nitrate, urea, have.
The leaching agent may have a chemical equivalent ratio of 2 to 25 to nickel and cobalt contained in the slurry.
The leaching can be carried out at a temperature ranging from 20 to < RTI ID = 0.0 > 99 C. < / RTI >
The nickel and cobalt recovery method of the present invention has the effect of lowering the recovery rate of iron from a low-quality raw material having a low content of nickel and cobalt, and recovering nickel and cobalt at a high recovery rate.
Hereinafter, preferred embodiments of the present invention will be described. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below.
Conventionally, the HPAL process or the Caron process has been carried out by recovering nickel and cobalt from a low-quality raw material having a low content of nickel and cobalt. However, the HPAL process has a problem that a process operation cost such as facility cost is high. There is a problem that the recovery rate of cobalt is low. However, the present invention can provide a nickel and cobalt recovery method which can be operated at a low cost and recovering nickel and cobalt from a low-quality raw material having a low content of nickel and cobalt, and recovering nickel and cobalt.
According to an embodiment of the present invention, there is provided a process for producing a reducing raw material, comprising the steps of: introducing a mixed raw material containing nickel cobalt-containing raw material and coal powder into a reducing furnace to obtain a reducing raw material; slurrying the reducing raw material in an inert atmosphere to prepare a slurry; And introducing the leaching agent into the slurry to obtain a leached product containing nickel and cobalt.
The nickel-cobalt-containing raw material which can be applied to the present invention is not particularly limited, but may be any as long as it contains nickel and cobalt. For example, limonite, saporrolite or a mixture thereof is preferable.
The content of the nickel cobalt-containing raw material varies depending on the kind, but usually the content of iron is as large as 40 to 50%, the content of nickel to be recovered is about 0.5 to 2.5% and the content of cobalt is about 0.05 to 0.25% Very few. The nickel and cobalt recovery method of the present invention can be effectively applied in recovering nickel and cobalt from low-quality raw materials having a low content of nickel and cobalt.
In recovering nickel and cobalt from the nickel-cobalt-containing raw material, in order to effectively reduce the nickel-cobalt-containing raw material in the reduction process described below, the drying process of drying the nickel-cobalt-containing raw material may be performed.
The drying process is preferably performed at a temperature ranging from 40 to 250 ° C, more preferably from 100 to 200 ° C. If the drying temperature is lower than 40 ° C, the adhesion water in the nickel-cobalt-containing raw material is not easily evaporated and the reduction and leaching process does not occur smoothly. If the drying temperature is more than 250 ° C, further drying is not performed, and unnecessary energy is consumed.
According to one embodiment of the present invention, it may include a reducing process for reducing nickel and cobalt contained in the nickel-cobalt-containing raw material. In the reduction process, nickel and cobalt may be reduced by mixing the nickel-cobalt-containing raw material with a coal powder as a reducing agent to prepare a mixed raw material, and then introducing the mixed raw material into a reducing furnace.
It is preferable to use coal powder as a reducing agent used for reducing nickel cobalt-containing raw materials. The coal powder is not particularly limited as long as it contains volatile matter and fixed carbon, but is preferably at least one selected from the group consisting of bituminous coal, semi-anthracite and anthracite. It is preferable that the content of the volatile matter contained in the coal is approximately 2 to 40% by weight, and the content of the fixed carbon is 10 to 60% by weight.
Since the coal has high activity even at a low temperature, the coal can be reduced even at a low temperature. That is, since the coal powder is used as the reducing agent for reducing the nickel-cobalt-containing raw material, the reduction process can be performed at a low temperature. Also, in the reduction process using coal powder, so-called nickel and cobalt preferential reduction, in which only the nickel and cobalt components contained in a small amount are preferentially reduced in the nickel-cobalt-containing raw material, may occur. Therefore, nickel and cobalt are reduced more than iron is reduced from nickel cobalt raw material. Therefore, nickel and cobalt can be recovered at a high recovery rate while lowering the recovery rate of iron from nickel and cobalt raw materials in a subsequent leaching step have.
The weight ratio of the nickel cobalt-containing raw material and the coal powder in the mixed raw material is preferably 100: 0.1 to 50, more preferably 100: 1 to 10. If the content of the coal powder is less than 0.1 part by weight with respect to 100 parts by weight of the nickel-cobalt-containing raw material, the reaction is completed without sufficiently reducing the amount of nickel and cobalt present in a trace amount to lower the recoverability of nickel and cobalt. If the amount is more than 50 parts by weight, excessive iron is reduced at the same time, so that not only the amount of acid consumed in the subsequent leaching step but also the amount of unwanted iron is increased.
It is preferable to use an atomized powder to perform efficient reduction and smooth leaching of the raw materials used for recovering nickel and cobalt. Therefore, the method may further include a step of pulverizing the mixed powder before the mixed powder containing the nickel-cobalt-containing raw material and the coal powder is put into the reducing furnace.
It is preferable that a reducing process is performed in an inert atmosphere when a reducing raw material is mixed with a raw material containing nickel cobalt-containing raw material and coal powder to perform a reducing process. The inert gas may be included to remove oxygen present in the reducing furnace during the reduction reaction. Such an inert gas is not particularly limited as long as it is not reactive, and examples thereof include helium, argon, carbon dioxide, nitrogen and the like.
Mixtures of nickel cobalt-containing raw materials and coal powders may be reduced in a reduction furnace. The temperature of the reducing furnace is preferably 250 to 800 ° C, and more preferably 300 to 650 ° C. If the temperature of the reducing furnace is lower than 250 캜, the reduction does not sufficiently take place and the recovery rate upon leaching into the acid solution in the subsequent step becomes low. On the other hand, the higher the reducing temperature, the faster the reaction rate. However, when the temperature of the reducing furnace exceeds 800 ° C., unnecessary energy is consumed.
By such a reaction, a raw material containing reduced nickel and cobalt can be obtained. The raw material containing the reduced nickel and cobalt is hereinafter referred to as a 'reducing raw material'.
The reducing raw material can be slurried using water to prepare a slurry. Preferably, the slurrying is carried out in an oxygen-free or inert atmosphere in which external air is blocked to prevent the reducing raw material from being reoxidized by oxygen. Since the reducing raw material obtained by reducing the nickel cobalt-containing raw material has high activity and a very high iron content, when the reducing raw material is extracted into the air after the reduction, reductant of the reducing raw material is reoxidized, Accelerated to have a fire hazard. Therefore, oxidation and ignition of the reducing raw material can be prevented by slurrying the reducing raw material with water.
In the slurrying step, the weight ratio of the reducing raw material and water is preferably 1: 1 to 25, more preferably 1: 1 to 4. If the weight ratio of water to the reducing raw material is less than 1, stirring in the leaching step is difficult to carry out, and if it is more than 25, the concentration of the solution after leaching becomes unfavorably low.
A leaching step may be performed in which the reducing raw material is made into a slurry and then an immersion agent is added to the slurry to ionize the nickel and cobalt contained in the reducing raw material in the slurry into nickel and cobalt ions. In the leaching step, the reducing raw material may be dissolved by adding an agitation agent to the slurry-reduced reducing raw material in the reactor and stirring the mixture.
The leaching agent used in the leaching step is not particularly limited, but an acid is preferably used. For example, at least one selected from the group consisting of sulfuric acid, sulfuric acid, hydrochloric acid, hydrochloric acid, nitric acid, nitric acid salt, hydrofluoric acid, hydrofluoric acid, phosphoric acid, phosphate, acetic acid, acetic acid salt, propionic acid, propionic acid salt, ammonium salt, aluminum nitrate, urea, desirable.
Preferably, the chemical agent has an equivalent chemical reaction ratio of 2 to 25, more preferably 5 to 15, to the nickel and cobalt contained in the slurry. If the chemical reaction equivalent ratio is less than 2, nickel and cobalt have a low leaching rate. If the chemical reaction equivalence ratio is more than 25, the leaching of the unwanted iron component increases and the consumption of the neutralizing agent increases in the subsequent process.
The leaching reaction using an acid is an exothermic reaction accompanied by an increase in temperature in the reactor. Therefore, the acid leaching reaction can be carried out even at room temperature. In particular, when the acid leaching reaction is carried out at a temperature of 20 ° C or more, good leaching efficiency can be obtained. Further, such an acid leaching reaction can be carried out by heating in an appropriate range, and when it is carried out by heating, the leaching rate can be further improved, and the leaching time can be shortened. The temperature at the time of heating may be suitably set in accordance with conditions of the reactor, and is not particularly limited. However, if the temperature exceeds 90 ° C during the leaching reaction, the cost of equipment for the leaching reaction may be increased. Therefore, it is preferable that the leaching is performed in a temperature range of 20 to 90 캜, and it is more preferably performed in a temperature range of 50 to 90 캜.
After the leaching reaction with an acid, a slurry in which a solution containing nickel and cobalt and a non-leached residue are mixed can occur. In order to separate the solution containing nickel and cobalt from the slurry, a conventional solid-liquid separation process may be used. The solid-liquid separation step may be performed using at least one selected from the group consisting of, for example, a filter press, a decanter, a drum filter, and a nasal filter. On the other hand, the impurities contained in the nickel and cobalt solution can be removed by a commonly known neutralization process. In addition, the final nickel and cobalt product recovery can be accomplished using hydroxide precipitation, sulfide precipitation, carbonic acid precipitation, oxidative precipitation, solvent extraction or crystallization processes.
Hereinafter, the present invention will be described more specifically by way of specific examples. The following examples are provided to aid understanding of the present invention, and the scope of the present invention is not limited thereto.
Example
The limonite ores were dried in a rotary kiln dryer at 150 ° C for 1 hour and then pulverized using a super-mill. After drying, the ground limonite ore was mixed with bituminous coal powder to prepare a mixed raw material, and the weight ratio of the limonite or bituminous coal to the mixed raw material was controlled to be 9: 1. The mixed raw materials were mixed using a ball mill for 1 hour. The ingredients were analyzed by inductively coupled plasma spectrometry (ICP) and the results are shown in Table 1. On the other hand, the components of bituminous coal were analyzed and shown in Table 2.
The mixed raw material was charged into a reducing furnace in a nitrogen atmosphere, heated to 600 캜 and maintained for 1 hour to prepare a reducing raw material. The reducing raw material was quenched with water, and the reducing raw material and water were mixed at a weight ratio of 1:10 to prepare a slurry. The slurry was heated to 80 DEG C, and 3.68 g of 97% sulfuric acid was blown into the slurry and reacted for 1 hour. The leach residue was separated from the leachate and analyzed by ICP. The concentrations of the components in the leach are shown in Table 3, and the leach rates of the components are calculated in Table 4.
As shown in Table 4, the leaching rate of iron is very low at 16%, but the leaching rate of cobalt and nickel is very high because the leaching rate of cobalt is 85% and the leaching rate of nickel is 96.2%.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, It will be obvious to those of ordinary skill in the art.
Claims (11)
Slurrying the reducing raw material in an inert atmosphere to produce a slurry; And
Adding an immersion agent to the slurry to obtain a leached product containing nickel and cobalt
≪ / RTI >
Further comprising the step of drying the nickel-cobalt-containing raw material.
Wherein the drying takes place in a temperature range of 40 to 250 < 0 > C.
Wherein the nickel-cobalt-containing raw material is limonite, saporitrite or a mixture thereof.
Wherein the coal powder is at least one selected from the group consisting of bituminous coal, semi-anthracite coal and anthracite coal.
Wherein the reducing furnace has a temperature of 250 to 800 占 폚.
Wherein the slurry comprises the reducing raw material and water, and the reducing raw material and water are in a weight ratio of 1: 1 to 25.
Wherein the precipitating agent is at least one selected from the group consisting of sulfuric acid, a sulfate, hydrochloric acid, hydrochloric acid, nitric acid, nitric acid salt, hydrofluoric acid, hydrofluoric acid, phosphoric acid, phosphate, acetic acid, acetic acid salt, propionic acid, propionic acid salt, ammonium salt, Nickel and cobalt recovery method.
Wherein the leaching agent has a chemical reaction equivalent ratio of 2 to 25 to nickel and cobalt contained in the slurry.
Wherein the leaching is carried out in a temperature range from 20 to < RTI ID = 0.0 > 99 C. < / RTI >
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020150122496A KR101664827B1 (en) | 2015-08-31 | 2015-08-31 | Method for recovering nickel and cobalt |
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| KR1020150122496A KR101664827B1 (en) | 2015-08-31 | 2015-08-31 | Method for recovering nickel and cobalt |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018117771A1 (en) * | 2016-12-23 | 2018-06-28 | 주식회사 포스코 | Method for recovering nickel and cobalt from nickel, iron, and cobalt-containing raw material |
| WO2019124977A1 (en) * | 2017-12-22 | 2019-06-27 | 주식회사 포스코 | Multistage reduction method for nickel ore |
| CN110114482A (en) * | 2016-12-23 | 2019-08-09 | 株式会社Posco | Method for recycling nickel and cobalt from the raw material containing nickel, iron and cobalt |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH11514705A (en) * | 1995-11-03 | 1999-12-14 | テクノロジカル リソーシズ プロプライエタリー リミテッド | A combined method for producing metals and metal alloys from metal oxide ores |
| KR101353721B1 (en) * | 2011-12-28 | 2014-01-21 | 재단법인 포항산업과학연구원 | Method for Recovering Ferro Nickel from Nickel Containing Raw Material |
| KR101403209B1 (en) * | 2012-12-21 | 2014-06-03 | 재단법인 포항산업과학연구원 | Method for recovering nickel from ni ore |
-
2015
- 2015-08-31 KR KR1020150122496A patent/KR101664827B1/en active IP Right Grant
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11514705A (en) * | 1995-11-03 | 1999-12-14 | テクノロジカル リソーシズ プロプライエタリー リミテッド | A combined method for producing metals and metal alloys from metal oxide ores |
| KR101353721B1 (en) * | 2011-12-28 | 2014-01-21 | 재단법인 포항산업과학연구원 | Method for Recovering Ferro Nickel from Nickel Containing Raw Material |
| KR101403209B1 (en) * | 2012-12-21 | 2014-06-03 | 재단법인 포항산업과학연구원 | Method for recovering nickel from ni ore |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018117771A1 (en) * | 2016-12-23 | 2018-06-28 | 주식회사 포스코 | Method for recovering nickel and cobalt from nickel, iron, and cobalt-containing raw material |
| CN110114482A (en) * | 2016-12-23 | 2019-08-09 | 株式会社Posco | Method for recycling nickel and cobalt from the raw material containing nickel, iron and cobalt |
| CN110114482B (en) * | 2016-12-23 | 2021-04-27 | 株式会社Posco | Process for the recovery of nickel and cobalt from a feedstock containing nickel, iron and cobalt |
| WO2019124977A1 (en) * | 2017-12-22 | 2019-06-27 | 주식회사 포스코 | Multistage reduction method for nickel ore |
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