CN102181665A - Method for keeping balance of sodium-magnesium-water system in technique for extracting nickel from lateritic nickel ore by wet process - Google Patents
Method for keeping balance of sodium-magnesium-water system in technique for extracting nickel from lateritic nickel ore by wet process Download PDFInfo
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Abstract
The invention discloses a method for keeping balance of a sodium-magnesium-water system in a technique for extracting nickel from lateritic nickel ore by a wet process, which is characterized by comprising the following steps: (a) dissolving nickelous hydroxide, which is obtained by carrying out alkali nickel precipitation on nickel sulfate leach liquor, in sulfuric acid; (b) extracting the nickel sulfate solution obtained in the step (a) with a P204 extractant to remove impurities, wherein P204 sodium soap is converted into nickel soap before removing the impurities; (c) extracting the nickel sulfate solution obtained in the step (b) with a P507 extractant to remove cobalt and magnesium, wherein P507 sodium soap is converted into nickel soap before removing the cobalt and magnesium; and (d) evaporating the anolyte, which is obtained by electrolyzing the nickel sulfate solution obtained in the step (c), thereby removing part of moisture. By using the method provided by the invention, the sodium, magnesium and water are balanced in the technique for extracting nickel from lateritic nickel ore by a wet process, so that the production can be carried out continuously, thereby increasing the recovery rate of nickel, lowering the treatment cost and having obvious economic efficiency.
Description
Technical field
The present invention relates to the hydrometallurgy field, relate in particular to a kind of red soil nickel ore wet method and carry and keep sodium, magnesium, aqueous systems equilibrated method in the nickel technology.
Background technology
The red soil nickel ore wet method carries that the main acid leaching process that adopts leaches nickel in the ore deposit in the flow process of nickel, no matter is to adopt normal pressure to leach or adopt high pressure to leach, and uses sulfuric acid as soaking the ore deposit agent mostly.For with the electrolytic nickel be product put forward the nickel flow process, single nickel salt behind leaching and preliminary chemical subtraction, concentration is very rare, nickel content often has only 1～5g/L, need precipitate-the molten step of acid improves the concentration of nickel in the solution, also contain iron in the nickel sulfate solution after precipitation-acid is molten, manganese, copper, zinc, calcium, impurity such as magnesium, adopt P204 solvent (di (isooctyl) phosphate) extraction process to come removal of impurities on the technology, come the separating nickel cobalt through P507 solvent (the own ester of 2-ethylhexyl phosphonic acid single 2-ethyl) extraction again, nickel sulfate solution is after treatment sent to electrowinning process and is produced metallic nickel.
In the process of heavy nickel, have part magnesium with the nickel coprecipitation, the molten back of acid magnesium dissolves with nickel and enters in the nickel sulfate solution, and in nickel electrowinning deposition process subsequently, magnesium can be stayed in the anolyte.Contain the vitriolic anolyte and must return the reaction of sour molten operation and nickel hydroxide, so, on the material flow of nickel, just constituted circulation to exhaust acid wherein.In working cycle, nickel is opened a way, and magnesium is closed circuit, and magnesium is constantly accumulation in system, causes the magnesium in the nickel sulfate solution cumulative, and then influences the electrolyting precipitation process of nickel, therefore need do the Balance Treatment of magnesium.
Nickel sulfate solution after molten to acid carries out P204 solvent extraction removal of impurities process, P204 organic phase after the back extraction must obtain regeneration through carrying out saponification reaction with dense sodium hydroxide solution, purpose is that the P204 organic phase is converted into sodium type salt from Hydrogen, so that the acidity of extractive reaction process nickel sulfate solution is stable.Be foreign metal positively charged ion and the exchange of the sodium ion on the P204 organic phase in the nickel sulfate solution on the P204 abstraction impurity removal process nature, the foreign metal positively charged ion enters organic phase, and sodium ion enters water.Equally, in the working cycle of anolyte, sodium also is closed circuit, and the sodium in the system also can accumulate gradually, so system also needs to do the Balance Treatment of sodium.
The nickel hydroxide that heavy nickel operation obtains contains big water gaging, in the molten process of acid, portion water enters the refining system, anolyte is also brought a considerable amount of moisture content into, also have various wash waters and technology reuse water also to enter system in addition, cause the nickel concentration of system thinning, therefore, system also needs to do the Balance Treatment of water.
At present, the accumulation problem that solution red soil nickel ore wet method is carried sodium, magnesium, water in the nickel system generally is nickel sulfate solution regularly to be extracted out carry out freezing treatment, wherein sodium, magnesium is separated out with the form crystallization of hydrated sulfate and obtain open circuit and remove, the processing that need stop production of this mode, process time is long, energy consumption is high, the loss of nickel is big.
Summary of the invention
In view of this, the purpose of this invention is to provide a kind of red soil nickel ore wet method carries and keeps sodium, magnesium, aqueous systems equilibrated method in the nickel technology.
Above-mentioned purpose realizes by following proposal:
A kind of red soil nickel ore wet method is carried and is kept sodium, magnesium, aqueous systems equilibrated method in the nickel technology, it is characterized in that, said method comprising the steps of:
A) to carry out acid with sulfuric acid molten for the nickel hydroxide that the single nickel salt leach liquor is obtained after with the heavy nickel of alkali;
B) the molten nickel sulfate solution that obtains of acid in the step a) is changed into nickel soap with the P204 soda soap through P204 extraction agent abstraction impurity removal before the removal of impurities;
C) nickel sulfate solution that step b) is obtained re-uses the extraction of P507 extraction agent except that cobalt magnesium, and elder generation enters extraction again except that cobalt, magnesium operation after the P507 soda soap is changed into the nickel soap before the extraction;
D) with c) anolyte after the nickel sulfate solution electrolysis that obtains of step evaporates and removes a part of moisture content.
According to aforesaid method, it is characterized in that, can be one of following with the alkali in the heavy nickel of alkali in the step a): sodium hydroxide, calcium hydroxide, magnesium hydroxide.
According to aforesaid method, it is characterized in that, the P204 soda soap changes into the nickel soap and is meant P204 soda soap and bright sulfur before extraction acid nickel solution is mixed in step b), by with bright sulfur acid nickel solution in the mode that exchanges of nickel ion form P204 nickel soap, enter P204 abstraction impurity removal operation again.
According to aforesaid method, it is characterized in that, after in step b), using P204 abstraction impurity removal, back extraction, earlier with the P204 organic phase of sodium hydroxide solution conversion after back extraction, make it be converted into the P204 soda soap, saponification degree must reach 60～70%, P204 soda soap and bright sulfur acid nickel solution is mixed change into P204 nickel soap then, and transformation efficiency must reach 60～90%.
According to aforesaid method, it is characterized in that, P507 soda soap in step c) changes into the nickel soap and is meant that P507 soda soap that extraction is preceding and bright sulfur acid nickel solution mix, by with bright sulfur acid nickel solution in the mode of nickel ion exchange form P507 nickel soap, drain wherein part sodium, and then enter the extraction of P507 extraction process and remove cobalt, magnesium.
According to aforesaid method, it is characterized in that, after in step c), using the P507 extraction except that cobalt, magnesium and after the back extraction, with the P507 organic phase of sodium hydroxide solution conversion after back extraction, make it be converted into the P507 soda soap, saponification degree must reach 60～70%, P507 soda soap and bright sulfur acid nickel solution is mixed change into P507 nickel soap then, and transformation efficiency must reach 60～90%.
According to aforesaid method, it is characterized in that described concentration of sodium hydroxide solution is 450～500g/L, the concentration of nickel is 10～100g/L in the bright sulfur acid nickel solution.
According to aforesaid method, it is characterized in that, in step d),, make nickel ion concentration bring up to 50～80g/L by the evaporation concentration anolyte.
Beneficial effect of the present invention: sodium, magnesium, water that the present invention puies forward in the nickel flow process red soil nickel ore wet method obtain balance, produce the rate of recovery carried out, improved nickel continuously, have reduced processing costs, economical efficiency is remarkable.
Description of drawings
Fig. 1 is the schema of the inventive method.
Embodiment
A kind of red soil nickel ore wet method is carried and is kept sodium, magnesium, aqueous systems equilibrated method in the nickel technology, it is characterized in that, said method comprising the steps of:
A) to carry out acid with sulfuric acid molten for the nickel hydroxide that the single nickel salt leach liquor is obtained after with the heavy nickel of alkali;
B) the molten nickel sulfate solution that obtains of acid in the step a) is changed into nickel soap with the P204 soda soap through P204 extraction agent abstraction impurity removal before the removal of impurities;
C) nickel sulfate solution that step b) is obtained re-uses the extraction of P507 extraction agent except that cobalt magnesium, and elder generation enters extraction again except that cobalt magnesium operation after the P507 soda soap is changed into the nickel soap before the extraction;
D) with c) anolyte after the nickel sulfate solution electrolysis that obtains of step evaporates and removes a part of moisture content.
Embodiment 1
Processing technological flow is seen Fig. 1, a kind of Indonesia produces the transition layer red soil nickel ore, contain Ni 1.5%, Fe 20%, Mg 12.5%, in the nickel sulfate solution after the leaching of normal pressure sulfuric acid, yellow modumite method removal of impurities, the solid-liquid separation, contains Ni 3.6g/L, Fe 0.18g/L, Mg 24g/L, this nickel sulfate solution heavy nickel of the sodium hydroxide solution of 30%wt, the nickel hydroxide that obtains is molten with vitriol oil acid, prepared nickel sulfate solution contains Ni 70g/L, Fe 0.01g/L, Na 32g/L, Mg 7.5g/L, earlier through P204 solvent extraction removal of impurities, to remove impurity such as wherein iron, manganese, copper, zinc.The manipulation of regeneration step of P204 is before the abstraction impurity removal: the sodium hydroxide solution of P204 organic phase after the back extraction and 500g/L concentration is mixed, carry out the P204 soda soapization, saponification degree with P204 in the determination of acid-basetitration organic phase, reach 60% and get final product phase-splitting, then organic phase and the bright sulfur acid nickel solution that contains Ni 10g/L are mixed, carry out the saponification of P204 nickel, sodium changes into the transformation efficiency of nickel in the mensuration organic phase, reaching 80% is phase-splitting, and the nickel organic phase of carrying after the conversion enters P204 abstraction impurity removal flow process.Contain through the nickel sulfate solution after the P204 solvent extraction removal of impurities: Ni 70g/L, Fe 0.001g/L, Na 36g/L, Mg 7.2g/L enters P507 collection cobalt separation of Cobalt and Nickel again.The manipulation of regeneration step of P507 is before the collection cobalt: the sodium hydroxide solution of P507 organic phase after the back extraction and 500g/L concentration is mixed, carry out the P507 soda soapization, measure the saponification degree of P507 in the organic phase, reaching 60% is phase-splitting, organic phase and the bright sulfur acid nickel solution that contains Ni 10g/L are mixed, carry out the saponification of P507 nickel, sodium changes into the transformation efficiency of nickel in the mensuration organic phase, reaching more than 60% is phase-splitting, and the nickel organic phase of carrying after the conversion enters P507 collection cobalt flow process.The nickel sulfate solution that obtains after P507 extracting and separating cobalt nickel contains: Ni 70g/L, and Na 37g/L, Mg 5g/L, magnesium has wherein reduced 30%, meets the technical requirements that electrowinning process is produced metallic nickel.Mode that soda soap by P204 and P507 transforms the nickel soap has reduced the sodium that extraction procedure is introduced in the nickel sulfate solution, and the sodium content in the nickel sulfate solution has obtained stablizing; Removed magnesium by P507 collection cobalt flow process, made part magnesium obtain open circuit, the Mg content in the nickel sulfate solution has obtained stable; Contain Ni 40g/L through the anolyte of electrowinning process, concentrate the part water of sloughing in the anolyte by consecutive evaporation, Ni concentration is brought up to 50g/L return sour molten operation again, the concentration of nickel sulfate after making acid molten has obtained stable.
Embodiment 2
Processing technological flow is with embodiment 1, red soil nickel ore, contain Ni 1.81%, Fe 22%, Mg 15.5%, in the nickel sulfate solution after the leaching of normal pressure sulfuric acid, yellow modumite method removal of impurities, the solid-liquid separation, contains Ni 4.3g/L, Fe 0.21g/L, Mg 26g/L, this nickel sulfate solution are with the heavy nickel of saturated aqua calcis, and the nickel hydroxide that obtains is molten with vitriol oil acid, prepared nickel sulfate solution contains Ni 72g/L, Fe 0.02g/L, Na 35g/L, Mg 8.5g/L, earlier through P204 solvent extraction removal of impurities, to remove impurity such as wherein iron, manganese, copper, zinc.The manipulation of regeneration step of P204 is before the abstraction impurity removal: the sodium hydroxide solution of P204 organic phase after the back extraction and 450g/L concentration is mixed, carry out the P204 soda soapization, saponification degree with P204 in the determination of acid-basetitration organic phase, reach 70% and get final product phase-splitting, then organic phase and the bright sulfur acid nickel solution that contains Ni 60g/L are mixed, carry out the saponification of P204 nickel, sodium changes into the transformation efficiency of nickel in the mensuration organic phase, reaching 85% is phase-splitting, and the nickel organic phase of carrying after the conversion enters P204 abstraction impurity removal flow process.Contain through the nickel sulfate solution after the P204 solvent extraction removal of impurities: Ni 72g/L, Fe 0.0005g/L, Na 36g/L, Mg 8.2g/L enters P507 collection cobalt separation of Cobalt and Nickel again.The manipulation of regeneration step of P507 is before the collection cobalt: the sodium hydroxide solution of P507 organic phase after the back extraction and 450g/L concentration is mixed, carry out the P507 soda soapization, measure the saponification degree of P507 in the organic phase, reaching 70% is phase-splitting, organic phase and the bright sulfur acid nickel solution that contains Ni 60g/L are mixed, carry out the saponification of P507 nickel, sodium changes into the transformation efficiency of nickel in the mensuration organic phase, reaching more than 85% is phase-splitting, and the nickel organic phase of carrying after the conversion enters P507 collection cobalt flow process.The nickel sulfate solution that obtains after P507 extracting and separating cobalt nickel contains: Ni 72g/L, and Na 38g/L, Mg 5.5g/L, magnesium has wherein reduced 35%, meets the technical requirements that electrowinning process is produced metallic nickel.Mode that soda soap by P204 and P507 transforms the nickel soap has reduced the sodium that extraction procedure is introduced in the nickel sulfate solution, and the sodium content in the nickel sulfate solution has obtained stablizing; Removed magnesium by P507 collection cobalt flow process, made part magnesium obtain open circuit, the Mg content in the nickel sulfate solution has obtained stable; Contain Ni 42g/L through the anolyte of electrowinning process, concentrate the part water of sloughing in the anolyte by consecutive evaporation, Ni concentration is brought up to 65g/L return sour molten operation again, the concentration of nickel sulfate after making acid molten has obtained stable.
Embodiment 3
Processing technological flow is with embodiment 1, red soil nickel ore, contain Ni 1.40%, Fe 17.5%, Mg 10.5%, in the nickel sulfate solution after the leaching of normal pressure sulfuric acid, yellow modumite method removal of impurities, the solid-liquid separation, contains Ni 3.2g/L, Fe 0.15g/L, Mg 22g/L, this nickel sulfate solution heavy nickel of the magnesium hydroxide solution of 80g/L, the nickel hydroxide that obtains is molten with vitriol oil acid, prepared nickel sulfate solution contains Ni 72g/L, Fe 0.02g/L, Na 35g/L, Mg 15g/L, earlier through P204 solvent extraction removal of impurities, to remove impurity such as wherein iron, manganese, copper, zinc.The manipulation of regeneration step of P204 is before the abstraction impurity removal: the sodium hydroxide solution of P204 organic phase after the back extraction and 500g/L concentration is mixed, carry out the P204 soda soapization, saponification degree with P204 in the determination of acid-basetitration organic phase, reach 65% and get final product phase-splitting, then organic phase and the bright sulfur acid nickel solution that contains Ni 100g/L are mixed, carry out the saponification of P204 nickel, sodium changes into the transformation efficiency of nickel in the mensuration organic phase, reaching 90% is phase-splitting, and the nickel organic phase of carrying after the conversion enters P204 abstraction impurity removal flow process.Contain through the nickel sulfate solution after the P204 solvent extraction removal of impurities: Ni 68g/L, Fe 0.001g/L, Na 30g/L, Mg 12g/L enters P507 collection cobalt separation of Cobalt and Nickel again.The manipulation of regeneration step of P507 is before the collection cobalt: the sodium hydroxide solution of P507 organic phase after the back extraction and 450g/L concentration is mixed, carry out the P507 soda soapization, measure the saponification degree of P507 in the organic phase, reaching 65% is phase-splitting, organic phase and the bright sulfur acid nickel solution that contains Ni 100g/L are mixed, carry out the saponification of P507 nickel, sodium changes into the transformation efficiency of nickel in the mensuration organic phase, reaching more than 90% is phase-splitting, and the nickel organic phase of carrying after the conversion enters P507 collection cobalt flow process.The nickel sulfate solution that obtains after P507 extracting and separating cobalt nickel contains: Ni 68g/L, and Na 30g/L, Mg 6.5g/L, magnesium has wherein reduced 45%, meets the technical requirements that electrowinning process is produced metallic nickel.Mode that soda soap by P204 and P507 transforms the nickel soap has reduced the sodium that extraction procedure is introduced in the nickel sulfate solution, and the sodium content in the nickel sulfate solution has obtained stablizing; Removed magnesium by P507 collection cobalt flow process, made part magnesium obtain open circuit, the Mg content in the nickel sulfate solution has obtained stable; Contain Ni 42g/L through the anolyte of electrowinning process, concentrate the part water of sloughing in the anolyte by consecutive evaporation, Ni concentration is brought up to 80g/L return sour molten operation again, the concentration of nickel sulfate after making acid molten has obtained stable.
Claims (8)
1. a red soil nickel ore wet method is carried and is kept sodium, magnesium, aqueous systems equilibrated method in the nickel technology, it is characterized in that, said method comprising the steps of:
A) to carry out acid with sulfuric acid molten for the nickel hydroxide that the single nickel salt leach liquor is obtained after with the heavy nickel of alkali;
B) the molten nickel sulfate solution that obtains of acid in the step a) is changed into nickel soap with the P204 soda soap through P204 extraction agent abstraction impurity removal before the removal of impurities;
C) nickel sulfate solution that step b) is obtained re-uses the extraction of P507 extraction agent except that cobalt magnesium, and elder generation enters extraction again except that cobalt, magnesium operation after the P507 soda soap is changed into the nickel soap before the extraction;
D) with c) anolyte after the nickel sulfate solution electrolysis that obtains of step evaporates and removes a part of moisture content.
2. method according to claim 1 is characterized in that, can be one of following with the alkali in the heavy nickel of alkali in the step a): sodium hydroxide, calcium hydroxide, magnesium hydroxide.
3. method according to claim 1, it is characterized in that, the P204 soda soap changes into the nickel soap and is meant that P204 soda soap that extraction is preceding and bright sulfur acid nickel solution mix in step b), by with bright sulfur acid nickel solution in the mode of nickel ion exchange form P204 nickel soap, enter P204 abstraction impurity removal operation again.
4. method according to claim 1, it is characterized in that, after in step b), using P204 abstraction impurity removal, back extraction, earlier with the P204 organic phase of sodium hydroxide solution conversion after back extraction, make it be converted into the P204 soda soap, saponification degree must reach 60～70%, P204 soda soap and bright sulfur acid nickel solution is mixed change into P204 nickel soap then, and transformation efficiency must reach 60～90%.
5. method according to claim 1, it is characterized in that, P507 soda soap in step c) changes into the nickel soap and is meant that P507 soda soap that extraction is preceding and bright sulfur acid nickel solution mix, by with bright sulfur acid nickel solution in the mode of nickel ion exchange form P507 nickel soap, drain wherein part sodium, and then enter the extraction of P507 extraction process and remove cobalt, magnesium.
6. method according to claim 1, it is characterized in that, after in step c), using the P507 extraction to remove cobalt, magnesium and back extraction, with the P507 organic phase of sodium hydroxide solution conversion after back extraction, make it be converted into the P507 soda soap, saponification degree must reach 60～70%, P507 soda soap and bright sulfur acid nickel solution is mixed change into P507 nickel soap then, and transformation efficiency must reach 60～90%.
7. according to claim 4 or 6 described methods, it is characterized in that described concentration of sodium hydroxide solution is 450～500g/L, the concentration of nickel is 10～100g/L in the bright sulfur acid nickel solution.
8. method according to claim 1 is characterized in that, in step d), by the evaporation concentration anolyte, makes nickel ion concentration bring up to 50～80g/L.
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Cited By (19)
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| CN102337403A (en) * | 2011-10-19 | 2012-02-01 | 江西稀有稀土金属钨业集团有限公司 | Online saponification system and process of extractant for Co-Ni separation |
| CN103074493A (en) * | 2013-02-20 | 2013-05-01 | 广西银亿科技矿冶有限公司 | Application of brucite to recovery of nickel cobalt |
| CN103468949A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Treatment method for scandium-containing cobalt nickel hydroxide |
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| 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 |
| CN103468948A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Method for comprehensive recycling of metals from scandium-containing cobalt nickel hydroxide |
| CN103468978A (en) * | 2013-08-15 | 2013-12-25 | 中国恩菲工程技术有限公司 | Method for extracting scandium from lateritic nickel ore sulfuric acid leaching solution |
| CN103484695A (en) * | 2013-08-15 | 2014-01-01 | 中国恩菲工程技术有限公司 | Treatment method for comprehensively recovering valuable elements from laterite-nickel ore |
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Application publication date: 20110914 |