CN101736157B - Process for absorbing and extracting valuable metal ions in leachate of laterite nickel ore by applying immobilized room temperature ionic liquid - Google Patents
Process for absorbing and extracting valuable metal ions in leachate of laterite nickel ore by applying immobilized room temperature ionic liquid Download PDFInfo
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- CN101736157B CN101736157B CN2009102426953A CN200910242695A CN101736157B CN 101736157 B CN101736157 B CN 101736157B CN 2009102426953 A CN2009102426953 A CN 2009102426953A CN 200910242695 A CN200910242695 A CN 200910242695A CN 101736157 B CN101736157 B CN 101736157B
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Abstract
The invention discloses a process for absorbing and extracting valuable metal ions in leachate of laterite nickel ore by applying immobilized room temperature ionic liquid, which comprises the following steps: 1) performing immobilization on the room temperature ionic liquid, namely 1-decyl-3-methylimidazole hexafluorophosphate or 1-decyl-3-methylimidazole tetrafluoroborate, immobilizing the roomtemperature ionic liquid to a porous solid absorption carrier to obtain an absorption reaction bed of the room temperature ionic liquid; 2) allowing a complex component, namely acid leachate obtainedby leaching the laterite nickel ore to pass through the absorption reaction bed for performing metal ion absorption at room temperature to extract the valuable metal ions in the leachate; and 3) achieving the purpose of performing elution and extraction on the metal ions by adjusting the acidity and flow rate of eluent. Through the process, an effective extraction process for the acid leachate ofthe laterite nickel ore can be established; the process fully uses low-grade mineral resources, improves the comprehensive utilization rate of the mineral resources, reduces environmental pollution, improves economic benefit, and can be applied to the development of the conventional low-grade non-ferrous metal mines in China.
Description
Technical field
The present invention relates to a kind of novel technology for extracting of red soil nickel ore acid leaching solution, particularly a kind of relating to ionic liquid at room temperature, form the adsorption of metal ions bed behind the carrier adsorption of immobilization, this adsorption bed can be to the valuable metal ions in the red soil nickel ore acid leaching solution (as Cu
2+, Ni
2+, Co
2+Deng) adsorb recovery.The invention belongs to metal ion solution-treated part in the hydrometallurgical technology research field.
Background technology
The leaching of mineral is important unit operations in the hydrometallurgy field, be the useful component in ore or the concentrate to be converted into soluble compound with chemical reagent, and optionally be dissolved out, obtain pregnant solution, realize useful component and impurity composition or gangue component separating process, finally reach the purpose that reclaims valuable metal.This method is applicable to handles ore and concentrate, unbalanced-ore, barren rock, slag and the various secondary material that metal content is low, dispersity is thin, component is complicated.Method is simple to operate, and the metal comprehensive recovery is higher.
The total resources of the nickel of China is 7,900,000 tons, presses the reserves basic calculation, and average resource more than 60% is the red soil nickel ore resource that is difficult to obtain economic utilization.The present situation of nickel resources poorness impels us to seek the difficult problem that a kind of novel industrial technology solves the red soil nickel ore utilization of resources.
Adopt biological metallurgy technical finesse red soil nickel ore, the metallurgical heterotrophic microorganism of screening high-performance bio, the selectivity organism that carries out red soil nickel ores such as nickel limonite or noumeite leaches and can obtain higher nickel, cobalt leaching yield.On production cost and processing power, be better than traditional pressurization leaching and high melt, reducing roasting-normal pressure ammonia and method such as soak.But characteristics such as the red soil nickel ore leach liquor exists, and potential of hydrogen height, complicated component, base metal ion content are low, doping organic phase and solid particulate adopt the chemical precipitation method rate of recovery low, and it is serious to carry phenomenon secretly, forms the harm of secondary solid pollutent composing environment; And it is many to adopt the common solvent extracting process to exist equipment (progression), take up an area of greatly, organic and inorganic reagent consumption is big, the more high defective of investment cost and production cost, and extraction agent self extraction efficiency is not high, seriously polluted, it is low to form production efficiency, the situation of industrial competition difference.Therefore, be necessary that the technology of seeking a kind of renewal handles the red soil nickel ore leach liquor.
Summary of the invention
The technology that the purpose of this invention is to provide valuable metal ions in a kind of immobilized room temperature ionic liquid adsorbing and extracting red soil nickel ore leach liquor, this technological operation is simple, the extraction efficiency height, and the operating time is short, realize multistage combination easily, have efficient, economical and environment amenable advantage.
For reaching the purpose of foregoing invention, the present invention by the following technical solutions:
The technology of valuable metal ions in this applying immobilized room temperature ionic liquid adsorbing and extracting red soil nickel ore leach liquor, it may further comprise the steps:
1), ionic liquid at room temperature 1-decyl-3-Methylimidazole hexafluorophosphate or 1-decyl-3-methyl imidazolium tetrafluoroborate are carried out the immobilization operation, is fixed on the porousness solid absorption carrier absorption reaction bed of ionic liquid at room temperature that obtained load;
2), red soil nickel ore is leached the complicated ingredient acid leaching solution obtain by the absorption reaction bed, carry out adsorption of metal ions under the normal temperature, the valuable metal ions in the extraction leach liquor;
3), reach the purpose that the metal ion wash-out comes together by regulating elutriant acidity and flow velocity.
Adsorption bed can be recycled within a certain period of time.
Described porousness solid absorption carrier is silica gel, montmorillonite or gac.
Valuable metal ions is Cu
2+, Ni
2+, Co
2+
Ionic liquid at room temperature (RTILs:Room temperat ure ionic liquids) is the fluid cpds of being made up of organic cation and organic or inorganic negatively charged ion fully under a class room temperature or the close temperature, belongs to salt, and fusing point is usually about below 100 ℃.Have nontoxic, do not have remarkable vapour pressure, environmentally friendly, do not have flammable, good conductivity and electrochemical window is wide, fusing point is low and liquid zone between the characteristics of wide, Heat stability is good, the multiple organism of solubilized and inorganics.Applied ionic liquid is water insoluble among the present invention, is slightly soluble in organic solvent, and liquid viscosity is higher, and this produce market is on sale.
This technology impregnated in carrier in the selected ionic liquid at room temperature under normal temperature condition, make ionic liquid loadedly on carrier by physical action, forms immobilized ionic liquid at room temperature.Again the immobilization ionic liquid is filled in the pipe reaction bed space, form the absorption reaction bed.With the low flow velocity of leach liquor by absorption reaction bed bed, make ionic liquid that valuable metal ions wherein is adsorbed in the load of bed institute mutually in.The elutriant that re-uses different acidity carries out the wash-out operation to the adsorption bed of having adsorbed metal ion, and metal ion is got back in the elutriant, makes metal ion obtain extracting and reclaims.
Advantage of the present invention is: technological operation is simple, the extraction efficiency height, and the operating time is short, realizes multistage combination easily, has efficient, economical and environment amenable advantage.
Description of drawings
Fig. 1: be process flow diagram of the present invention.
Fig. 2 a: the molecular structural formula of a kind of ionic liquid at room temperature 1-decyl-3-Methylimidazole hexafluorophosphate
Fig. 2 b: the molecular structural formula of a kind of ionic liquid at room temperature 1-decyl-3-methyl imidazolium tetrafluoroborate
Fig. 3: be formed absorption reaction bed synoptic diagram among the present invention.
Wherein, positively charged ion is 1-decyl-3-Methylimidazole; Negatively charged ion is hexafluoro-phosphate radical or tetrafluoroborate, is liquid under the room temperature, and each group all is ionic condition in the liquid.
Among Fig. 3,10 is fluid inlet, and 4 is reaction bed, and 11 is liquid outlet.
Embodiment
Among Fig. 1, (1) obtains ionic liquid at room temperature 1 through synthetic or outsourcing shown in operation 1, adopt 1-decyl-3-Methylimidazole hexafluorophosphate or 1-decyl-3-methyl imidazolium tetrafluoroborate.Its concrete molecular structural formula is shown in Fig. 2 a, b.
(2) shown in operation 2, select suitable inorganic porous property fixation support 2 for use, require this carrier acid-and base-resisting, and have certain mechanical strength.Selected solid support material is silica gel, montmorillonite and gac.
(3) shown in operation 3, inorganic fixation support be impregnated in the ionic liquid, left standstill 48 hours after fully stirring.The immobilized rate of ionic liquid is reached more than 75%.The ion liquid bed filler body that obtained load.
(4) shown in operation 4, with load ion liquid bed filler body be loaded in the reaction bed body 4.The bed body can adopt synthetic glass or stainless steel.The specific design parameter of bed body can be adjusted according to loadings size, filler particles granularity and leach liquor flow velocity.The granularity general requirement of filler is between 0.3～1cm.Its specific form as shown in Figure 3.
(5) shown in operation 5, red soil nickel ore resulting leach liquor 5 after acidity leaches is carried out ultimate analysis, measure valuable metal ions concentration wherein.
Total iron concentration must not be higher than 30g/L in the leach liquor.As go beyond the limit and to fall iron in advance and handle.Leach liquor acidity must not be higher than 20g/L.As go beyond the limit and then will carry out neutralizing treatment in advance.
(6) shown in operation 6, the mineral leach liquor is fed adsorption bed, reduce flow velocity as far as possible, prolonged the duration of contact between leach liquor and the adsorption stuffing.
Can be combined on the bed by physisorption through being adsorbed with 50～60% valuable metal ions.As not reaching the ionic adsorption rate of setting, adsorption operations can circulate.Leach liquor after absorption is discharged as surplus liquid.
(7) shown in operation 7, through adsorption process, the reaction bed 7 of valuable metal ions that obtained load.
(8) shown in operation 8, after adsorption process finishes, leach liquor aqueous phase institute huge legendary turtle metal ion part be enriched in the load of filling carrier institute ionic liquid mutually in.This moment can be in load in the reaction bed of valuable metal ions adverse current feed the water washing lotion, and the acidity value of adjustable water saving phase.Reduce flow velocity as far as possible, prolong the duration of contact between elutriant and the bed, and carry out the circulation between the eluting water phase.Through desorb 8 processes, make metal ion enter water.
(9) shown in operation 9, through above process, the valuable metal ions to aqueous phase carries out other art breading again, can obtain required valuable metal ions 9.
As shown in Figure 1, operation 3 is the load adsorption process of ionic liquid at room temperature and immobilization 3 carriers.
Embodiment 1
Select 1-decyl-3-Methylimidazole hexafluorophosphate for use, be immobilized onto on the montmorillonite carrier.After processing in 48 hours, immobilized rate can reach 77%.
Take the ore of cobalt nickel oxide acid leaching solution, its pH value is 3.5, and main component is Cu in this leach liquor
2+: 3.5g/l; Ni
2+: 1.2g/l; Co
2+: 0.6g/l; Fe
2+: 3.9g/l; Fe3
+: 9.5g/l.
At ambient temperature, leach liquor is splashed into the adsorption bed of vertical placement, collect surplus liquid in the bed bottom with the flow velocity of 5ml/min.Circular treatment 2 times.
Adopt ultraviolet spectrophotometry to analyze the adsorbed amount of metal ion of load filler in the adsorption bed.Calculating as can be known, the adsorption of metal ions rate is respectively: Cu
2+: 70%; Ni
2+: 81%; Co
2+: 84%; Fe
2+: 55%; Fe3
+: 62%.
The load filler of metal ion that taken out absorption in the adsorption bed places beaker.Adding volume ratio is the hydrochloric acid of 1: 1 2mol/L, fully stirs, and reaches the back extraction balance after about 3 minutes, and metallic nickel ions is at first come out by back extraction.In anti-raffinate, add volume ratio then and be 1: 1 3mol/L hydrochloric acid, make iron ion obtain back extraction.Remaining liq uses 1: 1 3mol/L hydrochloric acid to carry out back extraction again, makes cobalt ion enter water.Make adsorbed metal ion obtain progressively wash-out.
Analyze concentration of metal ions in the elutriant, calculate the eluting rate of metal ion, be respectively: Cu
2+: 86%; Ni
2+: 89%; Co
2+: 90%; Fe
2+: 85%; Fe3
+: 86%.The overall rate of recovery of metal ion is respectively: Cu
2+: 60%; Ni
2+: 73%; Co
2+: 75%; Fe
2+: 50%; Fe3
+: 57%.
Effect of the present invention is: by red soil nickel ore leaching liquid and adsorbed effect between the room temperature ionic liquid adsorbent bed, make the Cu in the leachate2+、Ni
2+、Co
2+The wash-out that obtains adsorbing with one by one Deng metal ion separates. Set up the new technology that the valuable metal ion effectively extracts in a kind of leaching of ores liquid.
Claims (1)
1. the technology of valuable metal ions in the applying immobilized room temperature ionic liquid adsorbing and extracting red soil nickel ore leach liquor, it is characterized in that: it may further comprise the steps:
1), ionic liquid at room temperature 1-decyl-3-Methylimidazole hexafluorophosphate or 1-decyl-3-methyl imidazolium tetrafluoroborate are carried out the immobilization operation, be fixed on the porousness solid absorption carrier, the absorption reaction bed of ionic liquid at room temperature that obtained load, described porousness solid absorption carrier is silica gel, montmorillonite or gac;
2), red soil nickel ore is leached the complicated ingredient acid leaching solution obtain by the absorption reaction bed, carry out adsorption of metal ions under the normal temperature, the valuable metal ions in the extraction leach liquor, described valuable metal ions is Cu
2+, Ni
2+, Co
2+
3), reach the purpose that the metal ion wash-out comes together by regulating elutriant acidity and flow velocity.
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| AU2011342380A1 (en) * | 2010-12-17 | 2013-07-25 | University Of South Australia | Extraction of metals |
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| CN115786703A (en) * | 2022-12-16 | 2023-03-14 | 吉林大学 | Method for extracting mineral ions by using inorganic porous material loaded with ionic liquid |
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| CN111151295A (en) * | 2019-12-31 | 2020-05-15 | 华南理工大学 | Surface modified composite carbon material for oxidative desulfurization and preparation method thereof |
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Effective date of registration: 20190625 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: YOUYAN ENGINEERING TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |
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Effective date of registration: 20210412 Address after: 101407 No.11, Xingke East Street, Yanqi Economic and Technological Development Zone, Huairou District, Beijing Patentee after: Youyan resources and Environment Technology Research Institute (Beijing) Co.,Ltd. Address before: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: YOUYAN ENGINEERING TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. |
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