CN105695740A - Method capable of improving acid resistance during reverse extraction of extraction agent containing pyridine carboxylic ester and dinonylnaphthalene sulfonic acid and application of method - Google Patents

Method capable of improving acid resistance during reverse extraction of extraction agent containing pyridine carboxylic ester and dinonylnaphthalene sulfonic acid and application of method Download PDF

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CN105695740A
CN105695740A CN201610072648.9A CN201610072648A CN105695740A CN 105695740 A CN105695740 A CN 105695740A CN 201610072648 A CN201610072648 A CN 201610072648A CN 105695740 A CN105695740 A CN 105695740A
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extraction
concentration
acid
back extraction
dinonylnaphthalene sulfonic
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胡慧萍
朱山
李吉源
陈启元
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Central South University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/40Mixtures
    • C22B3/406Mixtures at least one compound thereof being a heterocyclic compound
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y02P10/20Recycling

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Abstract

The invention discloses a method capable of improving acid resistance during reverse extraction of an extraction agent containing pyridine carboxylic ester and dinonylnaphthalene sulfonic acid and an application of the method. The application method is characterized in that the acid resistance during reverse extraction of the extraction agent can be obviously improved after trioctylphousphine oxide is added into the extraction agent containing pyridine carboxylic ester and dinonylnaphthalene sulfonic acid; moreover, nickel content in reverse extraction liquor can meet industrial needs of nickel electrolyte, the effect of simultaneously extracting Ni and Co from a multi-metal acid solution containing Fe, Ca, Mg, Co and Ni is not affected, and the removal effect on iron-calcium-magnesium impurities is not affected.

Description

A kind of improve containing picolinic acid ester and dinonylnaphthalene sulfonic acid extractant back extraction time acid proof method and application
Technical field
The present invention relates to Non-ferrous Metallurgy extracting process, acid proof method during the extractant back extraction that can be effectively improved containing picolinic acid ester and dinonylnaphthalene sulfonic acid (DNNSA) particularly to one and application。Also relating to can from the method extracting Co and Ni containing selectivity Fe, Ca, Mg, Co, Ni many metals acid solution simultaneously。
Background technology
Extractant containing picolinic acid ester and dinonylnaphthalene sulfonic acid (DNNSA) can be applicable to extract Ni and Co containing selectivity in Fe, Ca, Mg, Co, Ni many metals acid solution at present simultaneously。But extractant acid resistance is poor during back extraction, when back washing agent is H+Concentration more than 1mol/L (such as H+Concentration 2mol/L~4mol/L) sulphuric acid or just there is serious emulsion during hydrochloric acid solution, cause that back extraction can not point phase, it is impossible to meet commercial Application demand;As back washing agent H+When concentration is equal to 1mol/L, back extraction divides phase overlong time and Ni in strip liquor2+Cmax is 20.83g/L, it is impossible to meet nickel electrolyte to Ni2+The requirement of content。
There is presently no one can extract Ni and Co from containing selectivity Fe, Ca, Mg, Co, Ni many metals acid solution simultaneously, and make nickel content in strip liquor can meet the industrial requirements of nickel electrolyte, and acid proof method during containing picolinic acid ester and dinonylnaphthalene sulfonic acid extractant back extraction can be effectively improved。
Summary of the invention
Acid proof application process when it is an object of the invention to provide a kind of raising containing picolinic acid ester and dinonylnaphthalene sulfonic acid (DNNSA) extractant back extraction。
The present invention also aims to provide one can extract Ni and Co from containing selectivity Fe, Ca, Mg, Co, Ni many metals acid solution efficiently simultaneously, it is remarkably improved the extractant acid resistance at stripping process, and does not affect nickel cobalt extraction yield and ferrum calcium and magnesium impurities removing efficiency。
The present invention also can make Ni in strip liquor2+Content meets the industrial requirements of nickel electrolyte。
The application process of the present invention is in that, the application of trioctyl phosphine oxide, specifically adds trioctyl phosphine oxide (TOPO) in the extractant containing picolinic acid ester and dinonylnaphthalene sulfonic acid, improves acid resistance during extractant back extraction。
The present invention a kind of improves acid proof method during the extractant back extraction containing picolinic acid ester and dinonylnaphthalene sulfonic acid, it is extract in the stripping process of Ni and Co at many metals acid solution selectivity containing Fe, Ca, Mg, Co, Ni simultaneously, in the extractant containing picolinic acid ester and dinonylnaphthalene sulfonic acid, adds trioctyl phosphine oxide。
By above method, the method can significantly improve the extractant acid resistance at stripping process。
Extractant includes extractive reaction agent (main extractant and/or synergic reagent), diluent and/or regulator。In the method for the present invention, picolinic acid ester and dinonylnaphthalene sulfonic acid are main extractant and synergic reagent respectively。
The present invention to containing in the application process adding TOPO in picolinic acid ester and dinonylnaphthalene sulfonic acid extractant, could be applicable to copper, zinc, cadmium extraction process, and acid resistance when improving its back extraction。
The present invention extracts in the process of Ni and Co simultaneously, extracts and back extraction all carries out in the water bath with thermostatic control of 10~50 DEG C。H during back extraction+Concentration is sulphuric acid or the hydrochloric acid solution back extraction of 1.0~4.0mol/L。
The method of the present invention is that one can significantly improve acid proof method during containing picolinic acid ester and dinonylnaphthalene sulfonic acid extractant back extraction, improve acid resistance during extractant back extraction by addition TOPO, and make the nickel content in strip liquor meet the industrial requirements of nickel electrolyte。
Described picolinic acid ester structure isWherein substituent group is in ortho position or para-position。
The preferred version of the present invention includes:
The molar ratio range of picolinic acid ester and dinonylnaphthalene sulfonic acid is 1:1~4:1。
Organic facies involved in the present invention includes diluent (such as sulfonated coal wet goods), picolinic acid ester, dinonylnaphthalene sulfonic acid (DNNSA) and trioctyl phosphine oxide (TOPO)。
Trioctyl phosphine oxide and DNNSA molar ratio range are 0.5:1~5:1。More preferably trioctyl phosphine oxide is 1:1~3:1 with the molar ratio range of DNNSA。
Extraction phase ratio (O/A) is 1:2~2:1 (present invention compares the volume ratio referring to oil phase with aqueous phase)。Extract and carry out in 10~50 DEG C of waters bath with thermostatic control。
It is adopted as H during the back extraction of the present invention+The sulphuric acid of concentration 1.0~4.0mol/L or hydrochloric acid solution。Back extraction 20min in the water bath with thermostatic control of 10~50 DEG C。Back extraction compares (O/A) for 1:1~12:1。
The advantage of invention and good effect: (1) for the problem of acid resistance difference during containing picolinic acid ester and DNNSA extractant back extraction, adds acid resistance when TOPO is remarkably improved extractant back extraction in organic facies, shortens back extraction dramatically and divide the phase time;(2) toward containing after adding TOPO in picolinic acid ester and DNSSA extractant, nickel, cobalt metal can be extracted from the acid solution of the impurity such as iron content calcium and magnesium simultaneously, and not affect nickel cobalt extraction yield and ferrum calcium and magnesium impurities removing efficiency by this extractant effectively;(3) method of the present invention is also particularly suitable the H when back extraction+When concentration is more than 1mol/L, still can quickly carry out back extraction point phase, it is to avoid point phase overlong time。It is H referring to embodiments of the invention back washing agent+The sulphuric acid of concentration 1.0~4.0mol/L or hydrochloric acid solution。Adding after TOPO, the back extraction point phase time never adds the 867min (even cannot point phase) of TOPO and shortens to 2.5min~3min, highly shortened the back extraction point phase time;(4) present invention can make Ni in strip liquor2+And Co2+Concentration is respectively increased the about 80g/L after adding TOPO and about 5.4g/L from 20.83g/L and 2.08g/L when being not added with TOPO, that is:, after adding TOPO in the extractant containing picolinic acid ester and dinonylnaphthalene sulfonic acid, the nickel content in strip liquor can meet the industrial requirements of nickel electrolyte。。
In sum, toward containing picolinic acid ester and addition TOPO in DNNSA extractant, under the premise not affecting cobalt, nickel metal ion extraction rate and ferrum calcium and magnesium impurities removing efficiency, acid resistance during extractant back extraction can be significantly improved, it is greatly shortened the back extraction point phase time, and makes Ni in strip liquor2+Content brings up to the industrial requirements that can meet nickel electrolyte。
Detailed description of the invention
Following example are intended to that the invention will be further described, rather than limitation of the invention。
Comparative example 1
For do not add additive containing picolinic acid ester and dinonylnaphthalene sulfonic acid extractant, investigate back washing agent acidity and the back extraction phase acid proof impact of comparison extractant。
The extractant of picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) does not add additive, adopts sulfonated kerosene to be configured to extractant (i.e. oil phase) as diluent。The cobalt of impurity, the nickel acid solutions (namely by extraction aqueous phase) such as preparation iron content calcium and magnesium, wherein Ni2+Concentration is 2.5~4.0g/L, Co2+Concentration is 0.25~0.28g/L, Fe3+Concentration is 9.8~10.1g/L, Mg2+Concentration is 5.0~5.2g/L, Ca2+Concentration is 0.21~0.25g/L, and pH value is about 2。Extracting operation: by comparing 50ml oil phase and being joined in 250ml tool plug conical flask by extraction aqueous phase, then conical flask is put into vibration 20min in super constant temperature oscillator, pour standing point phase in separatory funnel after end into, measure the Ni in aqueous phase by EDTA compleximetry or ICP-AES method2+、Co2+、Fe3+、Ca2+、Mg2+Concentration, and the impurities removing efficiency (computing formula of impurities removing efficiency of the impurity such as extraction yield and ferrum calcium and magnesium of calculating cobalt nickelC in formulaMF、CNiFRepresent the concentration (g/L) of foreign metal ion M and nickel ion, C in feed liquid respectivelyMR、CNiRRepresent the concentration (g/L) of foreign metal ion M and nickel ion in strip liquor respectively)。Extract and back extraction condition: extraction phase ratio (O/A) is 1:2, extraction temperature 10~50 DEG C, extraction time 20min;H is adopted during back extraction+Concentration is the acid solution of 1.0~4.0mol/L back extraction 20min in 10~50 DEG C of waters bath with thermostatic control。Result is in Table 1。
Table 1 back washing agent acidity and back extraction phase comparison back extraction divide the impact of nickel cobalt ion concentration in phase time and strip liquor
Being found out by table 1, the extractant that picolinic acid ester and dinonylnaphthalene sulfonic acid form can extract Co and Ni to containing Fe, Ca, Mg, Co, Ni many metals acid solution simultaneously。Relatively Run1 and Run4, Run5 know, when back extraction compare (O/A) increase to 12:1 from 1:1 time, the back extraction point phase time is compared the 420min of 1:1 by back extraction increases to 867min when 5:1 is compared in back extraction, and cannot point phase when 12:1 is compared in back extraction;Back washing agent is H+The sulphuric acid of concentration 1.0mol/L or hydrochloric acid solution, when 5:1 is compared in back extraction, nickel cobalt ion concentration respectively 20.82g/L and 2.08g/L in strip liquor。
Embodiment 1
Fixing acid concentration (the H containing picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) extractant and back washing agent+Concentration is sulphuric acid or the hydrochloric acid solution of 1.0mol/L), extractant acid proof impact when the addition of investigation TOPO is on back extraction。
Toward containing picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) extractant add TOPO (molar ratio range with TOPO and the dinonylnaphthalene sulfonic acid related in " summary of the invention " is 1:1~3:1), sulfonated kerosene is adopted to be configured to extractant (i.e. oil phase) as diluent。The cobalt of impurity, the nickel acid solutions (namely by extraction aqueous phase) such as preparation iron content calcium and magnesium, wherein Ni2+Concentration is 2.5~4.0g/L, Co2+Concentration is 0.25~0.28g/L, Fe3+Concentration is 9.8~10.0g/L, Mg2+Concentration is 4.5~5.17g/L, Ca2+Concentration is 0.2~0.25g/L, and pH value is about 2。Extracting operation: by comparing 50ml oil phase and being joined in 250ml tool plug conical flask by extraction aqueous phase, then conical flask is put into vibration 20min in super constant temperature oscillator, pour standing point phase in separatory funnel after end into, measure the Ni in aqueous phase by EDTA compleximetry or ICP-AES method2+、Co2+、Fe3+、Ca2+、Mg2+Concentration, and calculate the impurities removing efficiency of the impurity such as extraction yield and ferrum calcium and magnesium of cobalt, nickel。Extract and back extraction condition: extracting and be in a ratio of 1:2, extraction temperature is 10~50 DEG C, extraction time 20min;H is adopted during back extraction+Concentration is the acid solution of 1.0mol/L back extraction 20min in 10~50 DEG C of waters bath with thermostatic control, and back extraction is in a ratio of 1:1。Result is in Table 2。
Back extraction is divided the impact of phase time by table 2TOPO addition
Found out by table 2, toward the acid resistance that can significantly improve containing addition TOPO in picolinic acid ester and dinonylnaphthalene sulfonic acid extractant during extractant back extraction, it is greatly shortened the back extraction point phase time, it is maintained with good result that cobalt and nickel are extracted simultaneously and the good removal effect to ferrum calcium and magnesium impurity, and along with TOPO and DNNSA mol ratio increases to 3:1 from 0:1, phase time back extraction time-division all shortens to 2.5min~3min。
Embodiment 2
Toward containing adding TOPO in picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) extractant, keeping TOPO and DNNSA mol ratio is 2:1, acid proof impact when investigating back washing agent acidity to extractant back extraction。
Toward containing picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) add TOPO (mol ratio of TOPO and dinonylnaphthalene sulfonic acid is 2:1), sulfonated kerosene is adopted to be configured to extractant (i.e. oil phase) as diluent。The cobalt of impurity, the nickel acid solutions (namely by extraction aqueous phase) such as preparation iron content calcium and magnesium, wherein Ni2+Concentration is 2.5~3.5g/L, Co2+Concentration is 0.25g/L, Fe3+Concentration is 9.8~10.1g/L, Mg2+Concentration is 5.0~5.2g/L, Ca2+Concentration is 0.2~0.25g/L, and pH value is about 2。Extracting operation: by comparing 50ml oil phase and being joined in 250ml tool plug conical flask by extraction aqueous phase, then conical flask is put into vibration 20min in super constant temperature oscillator, pour standing point phase in separatory funnel after end into, measure the Ni in aqueous phase by EDTA compleximetry or ICP-AES method2+、Co2+、Fe3+、Ca2+、Mg2+Concentration, and the impurities removing efficiency of the impurity such as extraction yield and ferrum calcium and magnesium of calculating cobalt nickel。Extract and back extraction condition: extract and be in a ratio of 1:2, extraction temperature 10~50 DEG C, extraction time 20min;H is adopted during back extraction+Concentration is the acid solution of 1.0~4.0mol/L back extraction 20min in 10~50 DEG C of waters bath with thermostatic control, and back extraction is in a ratio of 1:1。Result is in Table 3。
Back extraction is divided the impact of phase time by table 3 back washing agent acidity
Being found out by table 3, with the addition of the extractant of the picolinic acid ester of TOPO and dinonylnaphthalene sulfonic acid, along with back washing agent acidity increases, it is inconspicuous that back extraction divides the phase time to increase, and illustrates that the interpolation of TOPO can significantly improve acid resistance during the back extraction of extractant, and the back washing agent being suitable for is H+Concentration can hydrochloric acid from 1mol/L to 4mol/L or sulfuric acid solution。
Embodiment 3
Adding TOPO in the extractant containing picolinic acid ester and dinonylnaphthalene sulfonic acid, the mol ratio keeping TOPO and DNNSA is 2:1, and fixing back washing agent is H+The sulphuric acid of concentration 1.0mol/L or hydrochloric acid solution, investigate the impact of the picolinic acid ester relative quantity with the dinonylnaphthalene sulfonic acid extraction yield on cobalt nickel metal ion and ferrum calcium and magnesium impurity impurities removing efficiency。
Toward containing picolinic acid ester and dinonylnaphthalene sulfonic acid different mol ratio, (the molar concentration 0.45mol/L of fixing dinonyl sulfonic acid is constant, change the molar concentration of picolinic acid ester) extractant in add TOPO (mol ratio of TOPO and dinonylnaphthalene sulfonic acid is 2:1), adopt sulfonated kerosene to be configured to extractant (i.e. oil phase) as diluent。The cobalt of impurity, the nickel acid solutions (namely by extraction aqueous phase) such as preparation iron content calcium and magnesium, wherein Ni2+Concentration is 2.5~4.0g/L, Co2+Concentration is 0.25~0.28g/L, Fe3+Concentration is 9.8~10.1g/L, Mg2+Concentration is 5.0~5.2g/L, Ca2+Concentration is 0.22~0.25g/L, and pH value is about 2。Extracting operation: by comparing 50ml oil phase and being joined in 250ml tool plug conical flask by extraction aqueous phase, then conical flask is put into vibration 20min in super constant temperature oscillator, pour standing point phase in separatory funnel after end into, measure the Ni in aqueous phase by EDTA compleximetry or ICP-AES method2+、Co2+、Fe3+、Ca2+、Mg2+Concentration, and the impurities removing efficiency of the impurity such as extraction yield and ferrum calcium and magnesium of calculating cobalt nickel。Extract and back extraction condition: extract and be in a ratio of 1:2, extraction temperature 10~50 DEG C, extraction time 20min;H is adopted during back extraction+Concentration be the acid solution of 1.0mol/L at 10~50 DEG C of back extraction 20min, back extraction is in a ratio of 1:1。Result is in Table 4。
Table 4 adds the mol ratio of picolinic acid ester and the dinonylnaphthalene sulfonic acid impact on effect of extracting after TOPO
Being found out by table 4, along with the mol ratio of picolinic acid ester and dinonylnaphthalene sulfonic acid increases to 4:1 from 1:1, the impurities removing efficiency of the foreign metals such as the extraction yield of cobalt nickel and ferrum calcium and magnesium does not change substantially, and the back extraction point phase time does not change substantially yet。。
Embodiment 4
Adding TOPO in the extractant containing picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L), the mol ratio keeping TOPO and DNNSA is 2:1, and fixing back washing agent is H+The sulphuric acid of concentration 1.0mol/L or hydrochloric acid solution, investigate the extraction yield of extraction phase comparison cobalt nickel metal ion and the impact of the impurities removing efficiency of ferrum calcium and magnesium impurity。
Toward containing picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) extractant add TOPO (mol ratio of TOPO and dinonylnaphthalene sulfonic acid is 2:1), sulfonated kerosene is adopted to be configured to extractant (i.e. oil phase) as diluent。The cobalt of impurity, the nickel acid solutions (namely by extraction aqueous phase) such as preparation iron content calcium and magnesium, wherein Ni2+Concentration is 2.5~4.0g/L, Co2+Concentration is 0.25~0.28g/L, Fe3+Concentration is 9.8~10.1g/L, Mg2+Concentration is 5.0~5.2g/L, Ca2+Concentration is 0.2~0.25g/L, and pH value is about 2。Extracting operation: by comparing 50ml oil phase and being joined in 250ml tool plug conical flask by extraction aqueous phase, then conical flask is put into vibration 20min in super constant temperature oscillator, pour standing point phase in separatory funnel after end into, measure the Ni in aqueous phase by EDTA compleximetry or ICP-AES method2+、Co2+、Fe3+、Ca2+、Mg2+Concentration, and the impurities removing efficiency of the impurity such as extraction yield and ferrum calcium and magnesium of calculating cobalt nickel。Extract and back extraction condition: extraction temperature is 10~50 DEG C, extraction time 20min;H is adopted during back extraction+Concentration be the acid solution of 1.0mol/L at 10~50 DEG C of back extraction 20min, back extraction is in a ratio of 1:1。Result is in Table 5。
The impact of table 5 extraction phase comparison effect of extracting
Being found out by table 5, along with extraction phase is than increasing, the extraction yield of nickel cobalt increases, and the impurities removing efficiency of Fe, Ca, Mg impurity and back extraction point phase time do not change substantially。
Embodiment 5
Adding TOPO in the extractant that picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) form, the mol ratio keeping TOPO and DNNSA is 2:1, and fixing back washing agent is H+The sulphuric acid of concentration 4.0mol/L or hydrochloric acid solution, investigate the impact of cobalt, nickel concentration of metal ions in back extraction phase comparison strip liquor。
Toward containing picolinic acid ester (0.9mol/L) and dinonylnaphthalene sulfonic acid (0.45mol/L) extractant add TOPO (mol ratio of TOPO and dinonylnaphthalene sulfonic acid is 2:1), sulfonated kerosene is adopted to be configured to extractant (i.e. oil phase) as diluent。The cobalt of impurity, the nickel acid solutions (namely by extraction aqueous phase) such as preparation iron content calcium and magnesium, wherein Ni2+Concentration is 2.5~3.5g/L, Co2+Concentration is 0.25g/L, Fe3+Concentration is 9.8~10.1g/L, Mg2+Concentration is 5.0~5.2g/L, Ca2+Concentration is 0.21~0.25g/L, and pH value is about 2。Extracting operation: by comparing 50ml oil phase and being joined in 250ml tool plug conical flask by extraction aqueous phase, then conical flask is put into vibration 20min in super constant temperature oscillator, pour standing point phase in separatory funnel after end into, measure the Ni in aqueous phase by EDTA compleximetry or ICP-AES method2+、Co2+、Fe3+、Ca2+、Mg2+Concentration, and the impurities removing efficiency of the impurity such as extraction yield and ferrum calcium and magnesium of calculating cobalt nickel。Extract and back extraction condition: extract and be in a ratio of 1:2, extraction temperature 10~50 DEG C, extraction time 20min;H is adopted during back extraction+Concentration is that the acid solution of 4.0mol/L is at 10~50 DEG C of back extraction 20min。Result is in Table 6。
The impact of cobalt nickel concentration of metal ions in table 6 back extraction phase comparison strip liquor
Found out by table 6,12:1 is increased to from 1:1 along with back extraction is compared, cobalt in strip liquor, nickel metal ion concentration compare 6.30g/L and the 0.62g/L of 1:1 from back extraction, increase respectively to back extraction and compare 80.45g/L and the 5.41g/L of 12:1, and the back extraction point phase time does not change substantially。

Claims (10)

1. the application process of trioctyl phosphine oxide, it is characterised in that add trioctyl phosphine oxide in the extractant containing picolinic acid ester and dinonylnaphthalene sulfonic acid, improve acid resistance during extractant back extraction。
2. acid proof method during the extractant back extraction that can improve containing picolinic acid ester and dinonylnaphthalene sulfonic acid, it is characterized in that, to in the stripping process extracting Co and Ni containing Fe, Ca, Mg, Co and Ni many metals acid solution selectivity simultaneously, add trioctyl phosphine oxide to containing in the picolinic acid ester extractant with dinonylnaphthalene sulfonic acid。
3. method according to claim 2, it is characterised in that trioctyl phosphine oxide and dinonylnaphthalene sulfonic acid molar ratio range are 0.5:1~5:1。
4. method according to claim 3, it is characterised in that the molar ratio range of trioctyl phosphine oxide and DNNSA is 1:1~3:1。
5. method according to claim 2, it is characterised in that the molar ratio range of picolinic acid ester and dinonylnaphthalene sulfonic acid is 1:1~4:1。
6. method according to claim 2, it is characterised in that described picolinic acid ester has a structure in which;Wherein substituent group is in ortho position or para-position。
7. method according to claim 2, it is characterised in that during back extraction, adopts H+The sulphuric acid of concentration 1.0~4.0mol/L or hydrochloric acid solution carry out back extraction。
8. method according to claim 2, it is characterised in that the organic facies diluent extracted is sulfonated kerosene, and extraction phase is 1:2~2:1 than O/A。
9. method according to claim 2, it is characterised in that it is 1:1~12:1 that O/A is compared in back extraction。
10. the method according to any one of claim 2-9, it is characterised in that described many metals acid solution, Ni2+Concentration is 2.5~4.0g/L, Co2+Concentration is 0.25~0.28g/L, Fe3+Concentration is 9.8~10.1g/L, Mg2+Concentration is 4.5~5.2g/L, Ca2+Concentration is 0.2~0.25g/L。
CN201610072648.9A 2016-02-02 2016-02-02 Method capable of improving acid resistance during reverse extraction of extraction agent containing pyridine carboxylic ester and dinonylnaphthalene sulfonic acid and application of method Pending CN105695740A (en)

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CN108277365A (en) * 2018-02-05 2018-07-13 中南大学 The application of trialkyl naphthalene sulfonic acids, the synergic reagent comprising trialkyl naphthalene sulfonic acids and its preparation and application
CN108642283A (en) * 2018-05-25 2018-10-12 中南大学 A kind of nickel cobalt synergic reagent and its method detached with impurity extraction for nickel cobalt
GB2607991A (en) * 2021-06-11 2022-12-21 Johnson Matthey Plc A recycling method for battery and catalyst materials

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