CN113308603B - Treatment method of interphase dirt in nickel-cobalt metallurgy P204 extraction system - Google Patents
Treatment method of interphase dirt in nickel-cobalt metallurgy P204 extraction system Download PDFInfo
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- C22B23/00—Obtaining nickel or cobalt
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Abstract
The invention belongs to the technical field of extraction chemistry and chemical engineering, and particularly relates to a method for treating interphase dirt in a nickel-cobalt metallurgy P204 extraction system, which comprises the following steps: (1) collecting and pretreating interphase dirt: extracting organic matters containing interphase dirt generated by a nickel-cobalt P204 extraction system, and carrying out solid-liquid separation to obtain the interphase dirt and the entrained organic matters; (2) dispersing: adding ethanol into interphase dirt, heating to pulpify, and stirring; (3) and (3) precipitation: adding liquid caustic soda into the dispersed interphase dirt, standing for phase splitting, discharging bottom slurry, wherein the part which is not discharged is recycled mixed organic matter; (4) separation of mixed organic and ethanol: distilling the mixed organic matter to obtain distilled ethanol and separated organic matter; (5) and after separation, the organic matter is reused. The invention can recover the organic phase in the P204 interphase dirt, compared with the new extractant, the extraction performance of the recovered organic phase can be dissolved with the new extractant and the diluent, the extraction capability is not obviously reduced, and the organic phase can be returned to the system for use.
Description
Technical Field
The invention belongs to the technical field of extraction chemistry and chemical engineering, and particularly relates to a method for treating interphase dirt in a nickel-cobalt metallurgy P204 extraction system.
Background
With the rapid development of new energy vehicles, in the nickel-cobalt hydrometallurgy, the extraction technology is widely applied due to the advantages of high separation efficiency, large production capacity, good separation effect, high recovery rate, low reagent consumption, simple equipment, easy realization of automation and continuity in the production process and the like. The most commonly used extractant P204 for impurity removal in nickel and cobalt hydrometallurgy is easy to generate interphase dirt after long-term recycling, and comprises the following main components: high valence metal ion extract, silicon dioxide, inorganic silicate, colloidal ferric hydroxide, colloidal aluminum hydroxide, suspended particles and calcium sulfate crystals. The interphase dirt is mainly formed because the extractant simultaneously extracts trace high-valence (+ 3-valence and higher valence) metal ions in the extraction process, the ions are difficult to separate from the extractant by acid or saponification after being loaded with an organic phase, the trace high-valence ions are always enriched in the organic phase until high-valence metal ion complexes in the organic phase are saturated and then separated out, and the pasty interphase dirt is formed with solid suspended matters, colloidal ferric hydroxide, aluminum hydroxide, silicon dioxide and the like in the solution and is non-uniformly distributed between the aqueous phase and the organic phase. The interphase dirt can cause the serious emulsification phenomenon formed in the extraction process, cause the loss of the extracting agent, lead to the shutdown cleaning or the replacement in serious conditions, and is not beneficial to improving the production efficiency.
In order to slow down the precipitation rate of the interphase dirt and avoid frequently treating the interphase dirt, the following measures are generally adopted in the prior art: (1) removing impurities from the extraction stock solution in advance to reduce the content of high-valence metal ions and silicon in the extraction stock solution, thereby slowing down the processes of extraction, enrichment and saturation of the metal ions; (2) carry out the secondary filter to the extraction stoste before the extraction to reduce the content of suspended solid, use closed container in the operation process, avoid outside dust to get into the system, avoid the suspended solid to pollute organic and then accelerate the formation of filth. According to the above prior art, although the generation rate of the phase-to-phase contaminants can be slowed down in various ways, the phase-to-phase contaminants still need to be cleaned or treated regularly, and the treatment manner of the phase-to-phase contaminants also varies according to the specific components of the phase-to-phase contaminants. The interphase dirt treatment mode mainly comprises standing sedimentation in the use process of the P204 extractant, the method has long operation period and low separation efficiency, and the extraction condition needs to be adjusted according to the actual situation so as to ensure that the stability of an extraction system is not influenced. The method for treating the P204 interphase dirt in the new process for treating the interphase dirt generated by the P204 extraction system, which is published by the grant CN102676813B, is to separate an organic phase, a water phase and a solid phase in the P204 interphase dirt by using a high-speed centrifuge, wherein the separated waste residue has low oil content, high treatment efficiency and environmental friendliness, but is only limited to treating the interphase dirt caused by suspended particles in the P204. The process of generating interphase dirt for the extractant P204 used in the nickel-cobalt hydrometallurgy is generated from various reasons and long-term accumulation, so that most of the extractants have no targeted measures for recovering the organic phase therein.
In order to solve the defects of the prior art, the invention provides a method for treating interphase dirt in a nickel-cobalt metallurgy P204 extraction system, the method is simple and easy to treat the extractant interphase dirt, the recovered organic extraction effect after treatment is not obviously reduced, the added medicament can be recycled, and the method belongs to an environment-friendly technology.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for treating interphase dirt in a nickel-cobalt metallurgy P204 extraction system, which solves the problems that in the existing nickel-cobalt hydrometallurgy industry, the P204 extractant is used for a long time to generate the interphase dirt, so that the extraction capacity is reduced, and an organic phase is recovered from the interphase dirt without pertinence.
The technical scheme of the invention is as follows:
the method for treating interphase dirt in the nickel-cobalt metallurgical P204 extraction system comprises the following steps:
(1) collecting and pretreating interphase dirt: extracting organic matters containing interphase dirt generated by the nickel-cobalt extraction system, carrying out solid-liquid separation to obtain the interphase dirt and entrained organic matters, and returning the entrained organic matters to the system for use;
(2) dispersing: adding an ethanol solution into the interphase dirt, heating, stirring and slurrying to fully disperse the interphase dirt;
(3) and (3) precipitation: adding liquid alkali into the dispersed interphase sewage, heating, stirring, reacting to generate precipitate, standing for phase splitting, discharging the precipitate slurry, carrying out solid-liquid separation on the precipitate slurry to obtain a precipitated water phase and precipitate, wherein the precipitate is treated as hazardous waste, the precipitated water phase is treated as alkaline wastewater, and the part which is not discharged is recycled mixed organic;
(4) separation of mixed organic and ethanol: distilling the mixed organic matter to obtain distilled ethanol and separated organic matter;
(5) and (3) returning the separated organic matter to a system for use, specifically, organically merging the separated organic matter into a sodium soap section in an extraction process, and introducing the organic matter into a nickel soap section and an extraction section or directly introducing the organic matter into the extraction process for extraction impurity removal or separation of a nickel-cobalt system.
When interphase dirt in a nickel-cobalt metallurgy P204 extraction system is treated, the liquid-solid mass ratio of the ethanol solution to the interphase dirt is critical, and preferably, the liquid-solid mass ratio of the ethanol solution to the interphase dirt is 10-12: 1. When the liquid-solid mass ratio of the ethanol solution to the interphase dirt is lower than 10:1, the interphase dirt cannot be completely dispersed, part of visible pasty interphase dirt still exists after dispersion, the oil content of a precipitate formed after subsequent addition of liquid caustic soda for organic recovery is high, the precipitate is not easy to wash, and even the precipitate cannot be formed, when the liquid-solid mass ratio is higher than 12:1, the recovery cost of the ethanol is increased, when the liquid-solid mass ratio is 10-12:1, the interphase dirt and the ethanol solution form a uniform phase, and the oil content of the precipitate formed after addition of the liquid caustic soda is lower after filter pressing. The interphase dirt of the invention is a paste carrying part of organic dirt, contains part of organic and diluent, wherein the organic phase carries part of high-valence metal elements, the interphase dirt also contains precipitated calcium sulfate, high-valence metal ion extract and the like, is in a water-in-oil state, is an inhomogeneous multiphase mixture, has poor dispersibility, can not generate precipitate by directly adding liquid alkali, and further obtains a reusable organic phase, so the organic phase needs to be dispersed in advance, and ethanol is usually used as an organic solvent. The concentration of ethanol is not critical, and in order to avoid introducing excessive water phase and not increase the recovery amount of ethanol, the volume fraction of ethanol solution is preferably 70-99%.
In order to obtain a good dispersion effect, i.e., to obtain a homogeneous phase, it is preferable that the dispersion temperature in the step (2) of the present invention is 70 to 75 ℃. When the dispersion temperature is lower than 70 ℃, the dispersion effect of interphase dirt is poor, the oil content of precipitate generated after the subsequent addition of liquid caustic soda is influenced, and in order to obtain a better dispersion effect and reduce the volatilization of ethanol, the dispersion temperature is not higher than 75 ℃, so that in order to obtain a better dispersion effect, namely, a uniform phase, the dispersion temperature in the step (2) is preferably 70-75 ℃. In order to form a precipitate and thus to achieve separation of the organic phase from the interphase contaminant, the precipitation temperature in step (3) of the present invention is preferably 70 to 75 ℃. In the precipitation step of the step (3), when the recovered organic temperature is lower than 70 ℃, a precipitate cannot be formed, and an organic phase cannot be separated; when the temperature is higher than 70 ℃, a precipitate can be formed, and in order to reduce the volatilization of ethanol, the ethanol in the mixed organic is further recovered, and the reaction temperature is preferably 70-75 ℃.
Through multiple experiments, when the concentration of the liquid caustic soda is higher than 35% or lower than 10%, no precipitate can be formed in the step (3), and the organic matters cannot be recovered, so that the mass concentration of the liquid caustic soda is preferably 10% -35%, and after the liquid caustic soda is added into the dispersed interphase dirt, the mass of the sodium hydroxide is 5% -10% of that of the interphase dirt before dispersion.
In order to separate the ethanol from the extracting agent, and simultaneously the sulfonated kerosene (diluent) in the organic is not distilled out together with the ethanol, preferably, the distillation temperature in the step (4) is 95-150 ℃, and the distillation temperature in the invention is higher than the boiling point of the ethanol and lower than the boiling points of the sulfonated kerosene and the P204 extracting agent, so that the ethanol can be separated from the extracting agent, and simultaneously the kerosene in the organic is not distilled out together with the ethanol.
In the invention, when ethanol is not added for dispersion (or water is added or diluent kerosene is added), under the same conditions, the direct addition of liquid caustic soda can not generate precipitate and can not recover the organic matters in interphase dirt, the kerosene serving as an organic solvent and water serving as a non-organic solvent have no dispersion effect on P204 interphase dirt under the same conditions, and the interphase dirt which is not added with ethanol for dispersion can not form precipitate and can not further recover an organic phase when the liquid caustic soda is added under the same conditions; methanol is added into the P204 interphase dirt, the same dispersion effect as ethanol can be achieved under the same conditions, the methanol does not enter a water phase, but precipitation cannot be generated due to strong toxicity, volatility and low boiling point of the methanol, and 10% -35% of liquid alkali is added under the same conditions. The volatilization of the methanol causes the recovery rate of the methanol to be reduced, and causes the severe working environment and the health hazard to the operators, so the methanol is not selected for dispersion; when polymer alcohols such as n-propanol and isopropanol are added into the P204 interphase dirt, the dispersion can not be carried out under the same conditions, and after liquid alkali is added, the polymer alcohols such as n-propanol and isopropanol enter the water phase, so that the dispersion effect can not be achieved, and after the liquid alkali is added, the precipitate can not be generated to further separate the organic phase, and in order to carry out the next precipitation to separate the organic phase from the water phase, ethanol is selected as a dispersing agent.
From the physical property of ethanol, the ethanol can be originally used as an organic solvent, and can be mutually dissolved with water in any proportion, the conclusion is drawn according to the common general knowledge that after the ethanol solution is added, the ethanol should be distributed in a water phase and an organic phase, but the inventor finds through experiments that the ethanol and the water are added into interphase dirt, the mixture is fully mixed and then stands for phase separation, and the ethanol does not enter the water phase; adding ethanol into interphase dirt without adding water, and finding that the ethanol can uniformly disperse the interphase dirt to form a uniform phase, when liquid alkali is added, the ethanol can generate precipitate with the dispersed interphase dirt under a certain condition, then standing for phase separation and solid-liquid separation can remove the precipitate and a water phase, and the ethanol is volatile.
The mixed density of ethanol, P204 extractant and diluent is less than that of water and is insoluble in water phase, after dispersion and precipitation, ethanol is not discharged with water phase but remains in organic phase to obtain mixed organic matter, and the mixed organic matter is distilled to separate ethanol from diluent and extractant, the separated organic phase contains diluent and extractant, and the separated ethanol can be used as dispersant for several times + The theoretical consumption of the extraction solvent exceeds 100 percent, and the detection shows that the system is saponified by 100 percent by liquid caustic soda, but the extraction capacity of the extraction solvent after separation is not obviously reduced, which indicates that the essence of the extraction solvent is not changed.
Other most commonly used extracting agents P507 and C272 in nickel-cobalt metallurgy are mainly used for nickel-cobalt separation, and generally, solutions mainly containing nickel, cobalt and magnesium are extracted (the content of other impurities is very low), cobalt and magnesium are extracted, then segmented back extraction is carried out by controlling acidity, a nickel sulfate solution with low impurities is obtained after extraction, and a magnesium sulfate solution with impurities and a cobalt sulfate solution with low impurities are respectively obtained after back extraction. In the nickel-cobalt metallurgy industry, because the solution is usually required to be subjected to pre-impurity removal (such as removal of iron, aluminum, titanium, zirconium, calcium, zinc, manganese, copper and the like) before P507 and C272 are used, unless the content of impurities except nickel, cobalt and magnesium in the solution is very low, so that a nickel-cobalt solution with low impurities can be obtained in the next step, the methods adopted for impurity removal mainly comprise a chemical precipitation method, an adsorption method and an extraction method, wherein the extraction method is the most common pre-impurity removal method (as long as the P204 can extract almost all impurities) namely, a P204 extracting agent is adopted to extract and remove impurities from the nickel-cobalt solution, the impurities are stripped through fractional stripping, the raffinate is subjected to nickel-cobalt separation by using P507 or C272, because the content of impurities in the P507 and C272 extraction system is very low, the P204 does not need to be frequently treated with interphase impurities, the service cycle of the P204 is far longer than that of the P204, and the quantity of the impurities is very small, and the main substances in the interphase dirt are silicon dioxide, nickel hydroxide and the like, the nickel sulfate solution containing impurities and the silicon dioxide slag can be obtained by adding acid for dissolution and solid-liquid separation, the problem that the next step of treatment can be carried out only by dispersion does not exist, and the treatment of the liquid alkali does not have the same technical effect as the treatment of the liquid alkali.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. under the same condition, compared with the new extractant, the extraction performance of the organic phase separated by the method of the invention can dissolve the organic phase separated with the new extractant and the kerosene, the extraction capability is not obviously reduced compared with the new extractant, the organic phase can be returned to the system for use, and the extraction capability is obviously improved compared with the organic phase containing interphase dirt.
2. The method for treating interphase dirt in the nickel-cobalt metallurgy P204 extraction system can effectively recover the organic matters in the interphase dirt and reduce the loss of the extracting agent.
3. The organic matter recovered by the method of the invention is equivalent to 100% sodium soap, the hydrogen ion concentration of the organic matter is not required to be recovered, the organic matter can be directly used, and the processes of acid washing to regenerate an extracting agent and alkali saponification are not required.
4. The method has the advantages of simple operation, mild conditions, no toxicity of used medicaments and secondary utilization.
Drawings
FIG. 1 is a flow chart of a method for treating interphase contaminants in a nickel cobalt metallurgical P204 extraction system in an embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
100g of P204 nickel cobalt extraction system containing interphase dirt with the volume concentration of 25% organic is filtered at normal temperature to obtain 60.5g of interphase dirt. Adding 726.0g of ethanol solution with the volume fraction of 70% into interphase dirt, stirring and washing for 30min at 75 ℃, fully dispersing, adding 17.3g of liquid caustic soda with the mass concentration of 35% into a dispersed system, stirring and reacting for 30min, transferring to a separating funnel, standing and phase splitting, wherein the upper layer is mixed organic, the lower layer is precipitated slurry, discharging the lower layer precipitated slurry, carrying out solid-liquid separation on the lower layer precipitated slurry to obtain a precipitated aqueous phase and precipitate, wherein the precipitate is treated as hazardous waste, the precipitated aqueous phase is treated as alkaline wastewater, taking the upper layer mixed organic into a distillation flask, distilling for 2h at 95 ℃, returning ethanol after distillation to serve as a dispersing agent, and distilling the residual organic phase, namely separated P204 (kerosene containing a diluent, wherein the volume concentration of P204 is 25%).
After separation, P204 is mixed with new 25% P204 with the same volume, the saponification rate is 50%, and the nickel soap conditions are as follows: the nickel concentration of the nickel liquid before the nickel soap is 80.1g/L, the temperature of the nickel soap is 30 ℃, the time of the nickel soap is 15min, the ratio of the nickel soap to the nickel soap is 1:1, the nickel soap is grade 3, the nickel soap is used for extracting and removing impurities from the nickel sulfate solution containing impurities, and the extraction conditions are as follows: the temperature is 30 ℃, the phase ratio is 1:1, the single extraction time is 15min, and the cross-flow extraction is carried out for 3 times. And taking another 25% of new P204 with the same amount, and performing sodium soap (the mass concentration of liquid alkali is 30%, the temperature of the sodium soap is 30 ℃, the time of the sodium soap is 15min, the saponification rate is 50%), nickel soap and extraction conditions on the new P204 with the same organic phase after separation. After separation, the organic nickel soap nickel is loaded with 12.69g/L, the new organic nickel soap nickel is loaded with 12.75g/L, and the organic nickel soap nickel and the new organic nickel soap nickel are clear and have no interphase dirt in the saponification and extraction processes. The composition of the raffinate and the raffinate are shown in table 1.
Table 1 example 1 comparison of the effect of P204 extraction after separation with new 25% P204 extraction
In actual production, the separated part has less organic content, cannot drive the whole extraction system to run, often matches different manufacturers and new and old extractants for use, and thus the extraction capacity cannot be reduced after the two are mixed, the compatibility of the two is good, layering cannot occur, and the two are not compatible after mixing. Since the volume fraction of P204 used in the nickel-cobalt extraction system is usually 20% to 25%, and the separated organic phase contains kerosene and an extraction agent, in this embodiment, after being mixed with a new 25% organic phase of the same volume and uniformly mixed, the saponification rate of the separated organic phase is reduced from 100% to 50%, and then the organic phase is extracted and compared with a new organic phase with a saponification rate of 50% under the same conditions. As can be seen from table 1, the separated organic phase has the same ability of P204 to extract each metal ion under the same conditions as the new organic phase, and both saponification and extraction processes are clear and free from interphase contamination during the specific experiment. From the experiment of this example, it can be seen that: firstly, the separated organic can be determined to be completely soluble in new organic and diluent without the problem of phase separation and incompatibility; and secondly, proving that the extraction capacity of the separated organic phase and the separation effect on each metal ion are not reduced under the same condition, which shows that compared with the new organic phase, the extraction performance of the organic phase separated by the method of the invention can be dissolved with the new extractant and kerosene, and the extraction capacity is not obviously reduced.
Example 2
Taking 1kg of interphase dirt subjected to filter pressing by a P204 nickel-cobalt extraction system, adding 10kg of ethanol solution with the volume fraction of 99% into the interphase dirt, stirring and washing for 30min at 70 ℃, fully dispersing, adding 400.0g of caustic soda liquid with the mass concentration of 20% into the dispersed system, stirring and reacting for 40min, transferring into a separating funnel, standing for phase separation, taking the upper layer as a mixed organic matter, taking the lower layer as a precipitate slurry, discharging the lower layer precipitate slurry, carrying out solid-liquid separation on the lower layer precipitate slurry, obtaining a precipitated water phase and a precipitate, wherein the precipitate is treated as hazardous waste, treating the precipitated water phase as alkaline wastewater, taking the upper layer mixed organic matter into a distillation flask, distilling for 4h at 105 ℃, returning the distilled ethanol as a dispersing agent, and distilling the residual organic matter, namely the separated P204 (containing kerosene and P204 extracting agent).
After separation, P204 is mixed with new 25 percent P204, the saponification rate is controlled to be 60 percent, and the nickel soap conditions are as follows: the nickel concentration of the nickel liquid before the nickel soap is 80.1g/L, the temperature of the nickel soap is 30 ℃, the time of the nickel soap is 15min, the ratio of the nickel soap to the nickel soap is 1:1, the nickel soap is grade 3, the nickel soap is used for extracting and removing impurities from the nickel sulfate solution containing impurities, and the extraction conditions are as follows: the temperature is 30 ℃, the phase ratio is 1:1, the single extraction time is 15min, and the cross-flow extraction is carried out for 3 times. Taking new 25% P204, and extracting with sodium soap (30% of liquid alkali mass concentration, 30% of sodium soap temperature, 15min of sodium soap time, 60% of saponification rate), nickel soap under the same condition as the organic phase after separation. Both the saponification and extraction processes are clear and have no interphase dirt. Specifically, as shown in table 2.
Table 2 example 2 comparison of the effect of P204 extraction after separation with a new 25% P204 extraction
Example 3
500kg of interphase sewage after filter pressing of a P204 nickel-cobalt extraction system, adding 550kg of ethanol solution with the volume fraction of 95% into the interphase sewage, stirring for 1h at 72 ℃, fully dispersing, adding 250kg of caustic soda liquid with the mass concentration of 10% into the dispersed system, stirring for reaction for 1h, standing for phase separation, wherein the upper layer is a mixed organic matter, the lower layer is a precipitation slurry body, discharging the lower-layer precipitation slurry body, carrying out solid-liquid separation on the lower-layer precipitation slurry body to obtain a precipitated water phase and a precipitate, wherein the precipitate is treated as hazardous waste, the precipitated water phase is treated with alkaline wastewater, the upper-layer mixed organic matter is distilled for 4h at 150 ℃, the ethanol is returned to be used as a dispersing agent after distillation, and the residual organic matter is separated P204 (containing kerosene and P204 extracting agent).
After separation, P204 is mixed with new 25 percent P204, the saponification rate is controlled to be 40 percent, and the nickel soap conditions are as follows: the nickel concentration of the nickel liquid before the nickel soap is 80.1g/L, the temperature of the nickel soap is 30 ℃, the time of the nickel soap is 15min, the ratio of the nickel soap to the nickel soap is 1:1, the nickel soap is grade 2, the nickel soap is used for extracting and removing impurities from a nickel sulfate solution containing impurities, and the extraction conditions are as follows: the temperature is 30 ℃, the ratio is 1:1, the single extraction time is 15min, the organic phase is not changed, new extraction stock solution is used for extraction each time, and the extraction stage number is 3. Taking new 25% P204, and extracting with sodium soap (liquid alkali mass concentration 30%, sodium soap temperature 30 deg.C, sodium soap time 15min, saponification rate 40%), nickel soap under the same conditions as those after separation. Both the saponification and extraction processes are clear and have no interphase dirt. Specifically, the results are shown in Table 3.
Table 3 comparison of the effect of P204 after separation with the new 25% P204 extraction in example 3
As can be seen from the data in tables 1 to 3, the extraction performance of the organic phase separated by the method of the present invention is compared with that of the new organic phase, the separated organic phase can be dissolved with the new extractant and kerosene, and the extraction capacity is not significantly reduced, which indicates that the organic phase is successfully extracted from the interphase dirt by the method of the present invention.
In order to examine the main components of the interphase dirt, 100g of the interphase dirt in examples 1, 2 and 3 was respectively burned at a temperature higher than 400 ℃, and the main components precipitated after burning are shown in Table 4.
TABLE 4 main components and contents of the first precipitate after firing
In the field of nickel cobalt hydrometallurgy, nickel cobalt solution is usually subjected to impurity removal in advance, and then P204 is used for extraction impurity removal to remove impurities such as manganese, zinc, copper, calcium and the like. As can be seen from table 4, the main components of the P204 interphase contaminant are, in addition to the organic phase: the main reasons for precipitation of alkali sulfates or hydroxides of scandium, titanium, zirconium, chromium, iron, silicon, calcium, magnesium, and silica are: because the raw materials have more impurities or the auxiliary materials introduce the impurities, most of the impurities can be extracted and separated through P204, wherein scandium, titanium, zirconium, chromium and the like are difficult to be separated from the extracting agent through a back extraction means of nickel-cobalt hydrometallurgy after being extracted, so that the impurities are always enriched in an organic phase until a high-valence metal ion extract compound in the organic phase is saturated and then separated out, and then the impurities are agglomerated with solid suspended matters, colloidal ferric hydroxide, aluminum hydroxide, silicon dioxide and the like in the solution to form pasty interphase dirt. In combination with the data in tables 1-3, it is clear that the organic phase can be successfully extracted from the interphase contaminants by the process of the present invention.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (4)
1. The method for treating interphase dirt in a nickel-cobalt metallurgical P204 extraction system is characterized by comprising the following steps of:
(1) collecting and pretreating interphase dirt: extracting organic matters containing interphase dirt generated by a nickel-cobalt P204 extraction system, carrying out solid-liquid separation to obtain interphase dirt and entrained organic matters, and returning the entrained organic matters to the system for use;
(2) dispersing: adding an ethanol solution into interphase dirt, heating, stirring and slurrying to fully disperse the interphase dirt;
(3) and (3) precipitation: adding liquid alkali into the dispersed interphase dirt, heating, stirring, standing for phase splitting, discharging the precipitate slurry, performing solid-liquid separation on the precipitate slurry to obtain a precipitated water phase and a precipitate, and recycling the undischarged part of the mixed organic;
(4) separation of mixed organic and ethanol: distilling the mixed organic matter to obtain distilled ethanol and separated organic matter;
(5) returning the organic matter to the system for use after separation;
the liquid-solid mass ratio of the ethanol solution to interphase dirt is 10-12: 1;
in the step (3), after the liquid caustic soda is added into the dispersed interphase dirt, the mass of the sodium hydroxide is 5% -10% of that of the interphase dirt before dispersion;
the mass concentration of the liquid caustic soda in the step (3) is 10-35%.
2. The method for treating interphase contamination in a nickel cobalt metallurgy P204 extraction system as claimed in claim 1, wherein: the volume fraction of the ethanol solution is 70-99%.
3. The method for treating interphase contamination in a nickel cobalt metallurgical P204 extraction system as claimed in claim 1, wherein the dispersion temperature in step (2) and the precipitation temperature in step (3) are both 70-75 ℃.
4. The method for treating interphase contamination in a nickel cobalt metallurgy P204 extraction system as claimed in claim 1, wherein: the distillation temperature in the step (4) is 95-150 ℃.
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