CN105907964B - The separation method of vanadium, scandium, iron in a kind of acid solution - Google Patents
The separation method of vanadium, scandium, iron in a kind of acid solution Download PDFInfo
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- CN105907964B CN105907964B CN201610271343.0A CN201610271343A CN105907964B CN 105907964 B CN105907964 B CN 105907964B CN 201610271343 A CN201610271343 A CN 201610271343A CN 105907964 B CN105907964 B CN 105907964B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention relates to the separation method of vanadium, scandium, iron in a kind of acid solution.Its scheme is that red mud is carried out into the solution that salt Ore Leaching obtains containing vanadium, scandium, iron, the solution containing vanadium, scandium, iron is adjusted into pH value to 1.5 ~ 3.0 again, then resin adsorption operation is carried out, the vanadium ion in solution is set to be adsorbed on resin, and scandium, iron rule are stayed in solution, vanadium and scandium, the separating effect of iron are reached, vanadium adsorption rate is more than 99.5%, then resin containing vanadium carries out desorption operation and obtains rich vanadium liquid, 50 ~ 200 times of vanadium concentration enrichment.Scandium, ferrous solution are reduced and extracted operation again, scandium and iron in solution is efficiently separated, scandium extraction yield is more than 99%, rich scandium liquid, 10 ~ 50 times of scandium concentration enrichment are obtained as strip liquor back extraction organic phase containing scandium using sodium hydroxide solution.The present invention has the enrichment times of three metal ion species separation rates high, vanadium and scandium high, extraction and back extraction medicament kind is few and consumption is low, technical process is simple, maneuverable feature.
Description
Technical field
The invention belongs to metal ion technical field of wet metallurgy, and in particular to vanadium, scandium, the separation side of iron in a kind of acid solution
Method.
Background technology
Vanadium, scandium are important transition rare earth elements, are widely used in space flight due to its good physical and chemical performance, urge
Change, illuminating industry, alloy industry, ceramic material, catalytic chemistry, nuclear power industry and fuel cell etc..Red mud is bauxite production
The alkali solid discarded object produced in alumina process, is also a kind of secondary mineral resources containing various valuable metals.According to
Alum clay orefield and the difference of production technology, wherein a small amount of vanadium and scandium can be contained, extraction vanadium and scandium have great therefrom
Economic benefit and social effect.
At present, the method that vanadium and scandium are extracted from red mud is mainly acidleach (Jiang Pingguo, Liao Chun sends out from red mud salt acidleach
Go out in liquid to extract technical study [J] the China YouSe metallurgy 2012,1 of scandium: 66-68；The peaceful of Xue An, Chen Xiaohu, Tang Xiao
The process conditions and dynamics research [J] non-ferrous metals (Smelting Part) of Leaching of Scandium, 2010,2 in red mud: 51-54；King
Gram duty, Li Sheng tiger alumina laterite salt Ore Leaching reclaims experimental study [J] the rare metals and hard alloy of vanadium,
2012, 40 (6):5-8).Red mud by after salt Ore Leaching, vanadium and scandium can a large amount of dissolutions in solution, while the iron in red mud
Also can dissolution, this will influence the separation of vanadium, scandium and iron, in addition influence final products purity.At present, the separation on vanadium and scandium
It is use extraction operation more, by extractant and back washing agent not of the same race by obtaining rich vanadium liquid and richness after multitple extraction and back extraction
Scandium liquid (Li W, Zhang Y M, Liu T, et al. Comparison of ion exchange and solvent
extraction in recovering vanadium from sulfuric acid leach solutions of stone
coal [J]. Hydrometallurgy, 2013, 131-132: 1-7；Zeng L, Li Q Q, Xiao L S, et
al. A study of the vanadium species in an acid leach solution of stone coal
using ion exchange resin[J]. Hydrometallurgy, 2010, 105: 176-178；Tian Yanwen, Zhai Yu
Spring, Zhai Xiujing waits basic research [J] Northeastern University's journal (natural science edition) of P204 hydrochloric acid system extracting scandiums,
1998, 19(2): 162-165).But separation rate of vanadium and scandium is low during this, impurity iron can be produced sternly to its separating-purifying
The influence of weight is, it is necessary to multitple extraction and back extraction operation.
Therefore, use solvent-extracted method, the method to there is vanadium and scandium the separation of the element such as traditional vanadium, scandium, iron more
Low separation efficiency, impurity iron had a strong impact in vanadium, the effect of extracting of scandium, organic phase rich in three metal ion species, back extraction medicament
Species is more and the defect such as consumption big, complex technical process, operating difficulties.
The content of the invention
The purpose of the present invention is just being directed to the weak point in the presence of above-mentioned prior art and is providing one kind can be from acid
The method that vanadium, scandium, iron are efficiently separated in solution, the method has the enrichment times of three metal ion species separation rates high, vanadium and scandium
High, extraction and back extraction medicament kind is few and consumption is low, technical process is simple, maneuverable requirement.
The purpose of the present invention can be realized by subordinate's technical measures：
The method that the present invention is used is that red mud is adjusted through the solution containing vanadium, scandium, iron obtained by hydrochloric acid solution leaching
PH value carries out resin adsorption operation to 1.5 ~ 3.0, then by regulate pH value containing vanadium, scandium, ferrous solution, make vanadium in solution from
Son is adsorbed on resin, and scandium, iron rule are stayed in solution, reaches vanadium and scandium, the separating effect of iron, and then resin containing vanadium is solved
Inhale operation and obtain rich vanadium liquid.Scandium, ferrous solution are reduced and are extracted operation again so that scandium and iron in solution are effectively divided
From obtaining rich scandium liquid.
Specifically：Methods described comprises the steps：
A, will contain vanadium, scandium, iron acid solution be placed in tank diameter, be added dropwise over 1 ~ 5 mol/L sodium hydroxide solutions,
Temperature is that 20 ~ 40 DEG C and stirring intensity are to adjust solution ph to 1.5 ~ 3.0 under the conditions of 20 ~ 60r/min, and pH will be regulated afterwards
Value containing vanadium, scandium, iron solution for standby；
B, to step a obtained by the solution containing vanadium, scandium, iron for regulating pH value carry out resin adsorption operation；Step is such as
Under：The resin that will have been pre-processed is fitted into ion exchange column, is 10 ~ 20 in liquid-solid ratio ml/g:To ion exchange under conditions of 1
Poured into post regulate pH value containing vanadium, scandium, iron solution, open ion exchange column tapping valve, control adsorption time be 30 ~
60min, obtains resin containing vanadium and containing scandium, ferrous solution, and more than 99.5%, the adsorption rate of scandium and iron is both less than 0.5% to the adsorption rate of vanadium,
Ion exchange column tapping valve is closed, desorption operation is carried out to resin containing vanadium, by mass fraction for 4 ~ 8% sodium hydroxide solution falls
Enter in ion exchange column, liquid-solid ratio ml/g is 1:5 ~ 10, control desorption time for 180 ~ 360min, obtain rich vanadium liquid；
C, to step b obtained by reduced containing scandium, ferrous solution and extracted operation；Step is as follows：First containing scandium, iron
In solution by per 100ml correspondence 3 ~ 9g adding proportion add reducing agent, the reducing agent be sodium sulfite or sodium thiosulfate,
Then stirring 30 ~ 60min under the conditions of temperature is 20 ~ 40 DEG C and stirring intensity is 20 ~ 60r/min carries out reduction operation, afterwards
After by reduction containing scandium, ferrous solution and organic phase O/A volume ratios be 1:Mix under the conditions of 2 ~ 5, wherein organic phase is volume ratio
P507：TBP：Sulfonated kerosene=10：5：85 mixed solution, 5 ~ 10min, two-phase are shaken under the conditions of being 20 ~ 50 DEG C in extraction temperature
After separation, raffinate ferrous solution and organic phase containing scandium are obtained, the extraction yield of scandium is more than 99%, and the extraction yield of iron is less than 10%, then will
Organic phase containing scandium carries out back extraction operation, and it is 5 ~ 10 that will contain scandium organic phase with back washing agent O/A volume ratios:Mix under the conditions of 1, wherein instead
Extraction agent is the sodium hydroxide solution of 1 ~ 3mol/L, and 3 ~ 5min is shaken under the conditions of being 20 ~ 50 DEG C in back extraction temperature, after two-phase laminated flow,
Obtain rich scandium liquid.
Heretofore described acid solution is that red mud leaches gained through the hydrochloric acid solution that volume fraction is 5% ~ 20%, and wherein vanadium is dense
It is 50 ~ 100mg/L to spend, and scandium concentration is 5 ~ 15 mg/L, and ferric iron concentration is 1000 ~ 2000 mg/L.
Heretofore described resin preprocessing process is for first by D201,201*7 or D314 basic anionic resin with 1 ~ 3
Mol/L hydrochloric acid solutions soak 12 ~ 24h, are then 6.0 ~ 8.0 with distillation water wash resin to pH value, then by resin with 1 ~ 4
Mol/L sodium hydroxide solutions soak 12 ~ 24h, are then 6.0 ~ 8.0 with distillation water wash resin to pH value, and resin finally is used into 1
12 ~ the 24h of alcohol solution dipping of ~ 2 mol/L, is then 6.0 ~ 8.0 with distillation water wash resin to pH value.
Vanadium concentration is 2500 ~ 20000mg/L in products obtained therefrom richness vanadium liquid of the present invention, and scandium concentration is 50 ~ 750 in rich scandium liquid
mg/L。
Beneficial effects of the present invention are as follows：
Due to the present invention use salt Ore Leaching red mud, obtain containing other impurities species in vanadium, scandium, the acid solution of iron it is few and
Content is low, is conducive to vanadium, scandium, the separation of iron in acid solution, according to the thermodynamics collection of illustrative plates of vanadium, scandium, iron in solution, no matter in acid
Property, under neutrality, the pH value condition of alkalescence, scandium and iron are all in cationic form, and vanadium under conditions of pH value is more than 1.5 in it is cloudy from
Sub- form, therefore, use basic anionic resin with the vanadium ion in efficient absorption solution, and can not adsorb scandium ion and iron
Ion, thus realize that vanadium is separated with scandium, iron.Scandium and ferric iron by organic extractant phase, but can be moved according to extraction in solution
Mechanics study obtains the extraction ability of ferrous ion much smaller than ferric ion, therefore, using reducing agents pair such as sodium sulfites
Solution containing scandium, iron is reduced, and makes the ferric ion Restore All in solution into ferrous ion then organic using P507
Phase system is extracted, and the extraction yield of scandium is more than 99%, and the extraction yield of iron is less than 10%, then using sodium hydroxide solution as back extraction
Scandium in liquid back extraction organic phase, scandium concentration obtains 10 ~ 50 times of enrichment, and iron will not be stripped, and finally give rich scandium liquid.
Therefore, the present invention has the enrichment times of three metal ion species separation rates high, vanadium and scandium high, extraction and back extraction medicament
Species is few and consumption is low, technical process is simple, maneuverable feature.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Specific embodiment
The present invention is below with reference to embodiment（Accompanying drawing）It is further described：
It is now that the technical parameter Unify legislation involved by the specific embodiment of the invention is as follows to avoid repeated description：Institute
It is that red mud leaches gained through the hydrochloric acid solution that volume fraction is 5% ~ 20% to state acid solution, and wherein vanadium concentration is 50 ~ 100mg/L, scandium
Concentration is 5 ~ 15 mg/L, and ferric iron concentration is 1000 ~ 2000 mg/L.The resin preprocessing process is first by D201,201*7
Or the basic anionic resin such as D314 soaks 12 ~ 24h with 1 ~ 3 mol/L hydrochloric acid solutions, then with distillation water wash resin to pH
It is 6.0 ~ 8.0 to be worth, then resin is soaked into 12 ~ 24h with 1 ~ 4 mol/L sodium hydroxide solutions, then with distillation water wash resin extremely
PH value is 6.0 ~ 8.0, finally by the resin 12 ~ 24h of alcohol solution dipping of 1 ~ 2 mol/L, then uses distillation water wash resin
It is 6.0 ~ 8.0 to pH value.Repeated no more in specific embodiment.
Embodiment 1
Acid solution is placed in tank diameter, 1 ~ 2 mol/L sodium hydroxide solutions are added dropwise over, temperature be 20 ~ 40 DEG C and
Stirring intensity is to adjust solution ph to 1.5 ~ 1.8 under the conditions of 20 ~ 60r/min, regulate pH value containing vanadium, scandium, iron solution
It is standby；The solution containing vanadium, scandium, iron that pH value will be regulated carries out resin adsorption operation；The resin that will have been pre-processed loads ion
It is 10 ~ 12 in liquid-solid ratio ml/g in exchange column:Under conditions of 1 to poured into ion exchange column regulate pH value containing vanadium, scandium,
The solution of iron, opens ion exchange column tapping valve, and it is 30 ~ 60min control adsorption time, obtains resin containing vanadium and molten containing scandium, iron
Liquid, more than 99.5%, the adsorption rate of scandium and iron is both less than 0.2% to the adsorption rate of vanadium, closes ion exchange column tapping valve, resin containing vanadium
Desorption operation is carried out, by mass fraction for 4 ~ 8% sodium hydroxide solution is poured into ion exchange column, liquid-solid ratio ml/g is 1: 5~
7, control desorption time for 180 ~ 360min, rich vanadium liquid is obtained, vanadium concentration is 2500 ~ 8000mg/L in rich vanadium liquid；Scandium, iron will be contained
Solution is reduced and is extracted operation；First reduction is added in containing scandium, the solution of iron by the adding proportion of 3 ~ 5g of correspondence per 100ml
Agent, the reducing agent is sodium sulfite or sodium thiosulfate, and it is 20 ~ 60r/min with stirring intensity to be then 20 ~ 40 DEG C in temperature
Under the conditions of stir 30 ~ 60min carry out reduction operation, then by reduction after be in O/A volume ratios containing scandium, ferrous solution and organic phase
1:Mix under the conditions of 2 ~ 3, wherein organic phase is volume ratio P507：TBP：Sulfonated kerosene is 10：5：85 mixed solution, in extraction
Temperature is 5 ~ 10min of concussion under the conditions of 20 ~ 50 DEG C, after two-phase laminated flow, obtains raffinate ferrous solution and organic phase containing scandium, the extraction of scandium
Rate is more than 99%, and the extraction yield of iron is less than 10%, and then will contain scandium organic phase carries out back extraction operation, will contain scandium organic phase and back washing agent
O/A volume ratios are 5 ~ 6:Under the conditions of 1 mix, wherein back washing agent for 1 ~ 3mol/L sodium hydroxide solution, back extraction temperature be 20 ~
3 ~ 5min is shaken under the conditions of 50 DEG C, after two-phase laminated flow, rich scandium liquid is obtained.Scandium concentration is 50 ~ 250 mg/L in rich scandium liquid.
Embodiment 2
Acid solution is placed in tank diameter, 2 ~ 3 mol/L sodium hydroxide solutions are added dropwise over, temperature be 20 ~ 40 DEG C and
Stirring intensity is to adjust solution ph to 1.8 ~ 2.5 under the conditions of 20 ~ 60r/min, regulate pH value containing vanadium, scandium, iron solution
It is standby；The solution containing vanadium, scandium, iron that pH value will be regulated carries out resin adsorption operation；The resin that will have been pre-processed loads ion
It is 12 ~ 15 in liquid-solid ratio ml/g in exchange column:Under conditions of 1 to poured into ion exchange column regulate pH value containing vanadium, scandium,
The solution of iron, opens ion exchange column tapping valve, and it is 30 ~ 60min control adsorption time, obtains resin containing vanadium and molten containing scandium, iron
Liquid, more than 99.8%, the adsorption rate of scandium and iron is both less than 0.4% to the adsorption rate of vanadium, closes ion exchange column tapping valve, resin containing vanadium
Desorption operation is carried out, by mass fraction for 4 ~ 8% sodium hydroxide solution is poured into ion exchange column, liquid-solid ratio ml/g is 1: 7~
8, control desorption time for 180 ~ 360min, rich vanadium liquid is obtained, vanadium concentration is 8000 ~ 12000mg/L in rich vanadium liquid；To contain scandium,
Ferrous solution is reduced and is extracted operation；First added also by the adding proportion of 5 ~ 7g of correspondence per 100ml in containing scandium, the solution of iron
Former agent, the reducing agent is sodium sulfite or sodium thiosulfate, and 20 ~ 40 DEG C and stirring intensity are stirring under the conditions of 20 ~ 60r/min
30 ~ 60min carries out reduction operation, then by reduction after containing scandium, ferrous solution and organic phase O/A volume ratios be 1:3 ~ 4 conditions
Lower mixing, wherein organic phase are volume ratio P507：TBP：Sulfonated kerosene is 10：5：85 mixed solution, extraction temperature be 20 ~
5 ~ 10min is shaken under the conditions of 50 DEG C, after two-phase laminated flow, raffinate ferrous solution and organic phase containing scandium is obtained, the extraction yield of scandium is more than
99.2%, the extraction yield of iron is less than 8%, and then will contain scandium organic phase carries out back extraction operation, will contain scandium organic phase and back washing agent O/A bodies
Product is than being 6 ~ 8:Mix under the conditions of 1, wherein back washing agent is the sodium hydroxide solution of 1 ~ 3mol/L, be 20 ~ 50 DEG C in back extraction temperature
Under the conditions of shake 3 ~ 5min, after two-phase laminated flow, obtain rich scandium liquid, in rich scandium liquid scandium concentration be 250 ~ 500 mg/L.
Embodiment 3
Acid solution is placed in tank diameter, 3 ~ 5 mol/L sodium hydroxide solutions are added dropwise over, temperature be 20 ~ 40 DEG C and
Stirring intensity is to adjust solution ph to 2.5 ~ 3.0 under the conditions of 20 ~ 60r/min, regulate pH value containing vanadium, scandium, iron solution
It is standby；The solution containing vanadium, scandium, iron that pH value will be regulated carries out resin adsorption operation；The resin that will have been pre-processed loads ion
It is 15 ~ 20 in liquid-solid ratio ml/g in exchange column:Under conditions of 1 to poured into ion exchange column regulate pH value containing vanadium, scandium,
The solution of iron, opens ion exchange column tapping valve, and it is 30 ~ 60min control adsorption time, obtains resin containing vanadium and molten containing scandium, iron
Liquid, more than 99.9%, the adsorption rate of scandium and iron is both less than 0.5% to the adsorption rate of vanadium, closes ion exchange column tapping valve, resin containing vanadium
Desorption operation is carried out, by mass fraction for 4 ~ 8% sodium hydroxide solution is poured into ion exchange column, liquid-solid ratio ml/g is 1: 8~
10, control desorption time for 180 ~ 360min, rich vanadium liquid is obtained, vanadium concentration is 12000 ~ 20000mg/L in rich vanadium liquid.To contain
Scandium, ferrous solution are reduced and are extracted operation；First add by the adding proportion of 7 ~ 9g of correspondence per 100ml in containing scandium, the solution of iron
Enter reducing agent, the reducing agent is sodium sulfite or sodium thiosulfate, then temperature be 20 ~ 40 DEG C and stirring intensity be 20 ~
Under the conditions of 60r/min stir 30 ~ 60min carry out reduction operation, then by reduction after containing scandium, ferrous solution and organic phase in O/A
Volume ratio is 1:Mix under the conditions of 4 ~ 5, wherein organic phase is volume ratio P507：TBP：Sulfonated kerosene is 10：5：85 mixing is molten
Liquid, 5 ~ 10min is shaken under the conditions of being 20 ~ 50 DEG C in extraction temperature, after two-phase laminated flow, obtains raffinate ferrous solution and organic containing scandium
Phase, the extraction yield of scandium is more than 99.5%, and the extraction yield of iron is less than 6%, and then will contain scandium organic phase carries out back extraction operation, and will contain scandium has
Machine phase is 8 ~ 10 with back washing agent O/A volume ratios:Mix under the conditions of 1, wherein back washing agent is the sodium hydroxide solution of 1 ~ 3mol/L,
Back extraction temperature be 20 ~ 50 DEG C under the conditions of shake 3 ~ 5min, after two-phase laminated flow, obtain rich scandium liquid, in rich scandium liquid scandium concentration be 500 ~
750 mg/L。
Therefore, the present invention has the enrichment times of three metal ion species separation rates high, vanadium and scandium high, extraction and back extraction medicament
Species is few and consumption is low, technical process is simple, maneuverable feature.
Claims (3)
1. vanadium, scandium, the separation method of iron in a kind of acid solution, it is characterised in that：Methods described comprises the steps：
A, will contain vanadium, scandium, iron acid solution be placed in tank diameter, 1 ~ 5 mol/L sodium hydroxide solutions are added dropwise over, in temperature
For 20 ~ 40 DEG C and stirring intensity are to adjust solution ph to 1.5 ~ 3.0 under the conditions of 20 ~ 60r/min, pH value will be regulated afterwards
Containing vanadium, scandium, iron solution for standby；The acid solution is that red mud leaches gained through the hydrochloric acid solution that volume fraction is 5% ~ 20%, its
Middle vanadium concentration is 50 ~ 100mg/L, and scandium concentration is 5 ~ 15 mg/L, and ferric iron concentration is 1000 ~ 2000 mg/L；
B, to step a obtained by the solution containing vanadium, scandium, iron for regulating pH value carry out resin adsorption operation；Step is as follows：Will
The resin for having pre-processed is fitted into ion exchange column, is 10 ~ 20 in liquid-solid ratio ml/g:Fallen in ion exchange column under conditions of 1
Enter to regulate pH value containing vanadium, scandium, iron solution, open ion exchange column tapping valve, control adsorption time be 30 ~ 60min, obtain
To resin containing vanadium and containing scandium, ferrous solution, more than 99.5%, the adsorption rate of scandium and iron is both less than 0.5% to the adsorption rate of vanadium, closes ion
Exchange column tapping valve, desorption operation is carried out to resin containing vanadium, by mass fraction for 4 ~ 8% sodium hydroxide solution pours into ion friendship
Change in post, liquid-solid ratio ml/g is 1:5 ~ 10, control desorption time for 180 ~ 360min, obtain rich vanadium liquid；
C, to step b obtained by reduced containing scandium, ferrous solution and extracted operation；Step is as follows：First in the solution containing scandium, iron
In by per 100ml correspondence 3 ~ 9g adding proportion add reducing agent, the reducing agent be sodium sulfite or sodium thiosulfate, then
Stirring 30 ~ 60min under the conditions of temperature is 20 ~ 40 DEG C and stirring intensity is 20 ~ 60r/min carries out reduction operation, afterwards will also
After original containing scandium, ferrous solution and organic phase O/A volume ratios be 1:Mix under the conditions of 2 ~ 5, wherein organic phase is volume ratio P507：
TBP：Sulfonated kerosene=10：5：85 mixed solution, 5 ~ 10min, two-phase laminated flow are shaken under the conditions of being 20 ~ 50 DEG C in extraction temperature
Afterwards, raffinate ferrous solution and organic phase containing scandium are obtained, the extraction yield of scandium is more than 99%, and the extraction yield of iron is less than 10%, then will contain scandium
Organic phase carries out back extraction operation, and it is 5 ~ 10 that will contain scandium organic phase with back washing agent O/A volume ratios:Mix under the conditions of 1, wherein back washing agent
It is the sodium hydroxide solution of 1 ~ 3mol/L, 3 ~ 5min is shaken under the conditions of being 20 ~ 50 DEG C in back extraction temperature, after two-phase laminated flow, obtains
Rich scandium liquid.
2. vanadium, scandium, the separation method of iron in acid solution according to claim 1, it is characterised in that：The resin pretreatment
Process is for first by D201,201*7 or D314 basic anionic resin immersion of 1 ~ 3 mol/L hydrochloric acid solutions 12 ~ 24h, Ran Houyong
Distillation water wash resin to pH value is 6.0 ~ 8.0, then resin is soaked into 12 ~ 24h with 1 ~ 4 mol/L sodium hydroxide solutions, then
It is 6.0 ~ 8.0 with distillation water wash resin to pH value, finally by the resin 12 ~ 24h of alcohol solution dipping of 1 ~ 2 mol/L, so
It is afterwards 6.0 ~ 8.0 with distillation water wash resin to pH value.
3. vanadium, scandium, the separation method of iron in acid solution according to claim 1, it is characterised in that：Products obtained therefrom richness vanadium liquid
Middle vanadium concentration is 2500 ~ 20000mg/L, and scandium concentration is 50 ~ 750 mg/L in rich scandium liquid.
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| CN106629809B (en) * | 2016-12-20 | 2022-09-16 | 攀枝花市精研科技有限公司 | Method for purifying coarse scandium oxide |
| CN109437463B (en) * | 2018-12-29 | 2023-09-12 | 江苏卓博环保科技有限公司 | Advanced treatment and recycling device for stone coal blank roasting vanadium extraction high-salt wastewater and using method |
| CN111945018B (en) * | 2020-09-15 | 2022-11-11 | 昆明理工大学 | Method for treating arsenic in arsenic-containing solution by using anion resin and red mud |
| CN112941327B (en) * | 2021-03-09 | 2022-06-10 | 河南理工大学 | Method for selectively separating vanadium and iron from red mud |
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| CN100549193C (en) * | 2007-12-08 | 2009-10-14 | 中国铝业股份有限公司 | From red mud, extract the method for metal scandium, titanium |
| CN101696473A (en) * | 2009-10-23 | 2010-04-21 | 陕西正道投资有限公司 | Process for extracting vanadium from stone coal by acid method for performing curing pretreatment on raw ore |
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