CN106350671B - A kind of method of purification enrichment vanadium in pickle liquor from bone coal - Google Patents
A kind of method of purification enrichment vanadium in pickle liquor from bone coal Download PDFInfo
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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
- 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
- C22B3/28—Amines
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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
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3842—Phosphinic acid, e.g. H2P(O)(OH)
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- 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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Abstract
The present invention relates to a kind of method of purification enrichment vanadium in pickle liquor from bone coal.Its technical solution is：Calcareous material is added in bone coal pickle liquor and adjusts pH value, separation of solid and liquid, obtains neutralizing slag and neutralizer；Iron powder or sodium sulfite are added into the neutralizer, adds salt of weak acid, obtains extraction stoste.The extraction stoste is through being obtained by extraction load organic phases and raffinate, and the load organic phases are washed to obtain washing back loading organic phase, and the washing back loading organic phase is stripped to obtain lean organic phase and rich vanadium liquid；Extraction is returned after the lean organic phase regeneration treatment.The present invention has the characteristics that the short pH stable of the solution in kind of extraction process, extraction series, vanadium and plurality of impurity ions good separating effect and rich vanadium liquid impurity less.
Description
Technical field
The invention belongs to purification enrichment vanadium technical field.More particularly in a kind of pickle liquor from bone coal purification enrichment vanadium side
Method.
Background technology
Bone coal, which is that China is peculiar, contains vanadium resource, the main preservation of vanadium in bone coal in mica group aluminium silicate mineral lattice,
While vanadium is extracted from bone coal, silicate mineral is destructurized, and aluminium, iron, phosphorus etc. are also leached at the same time, complicated from more impurity
Purification enrichment vanadium is the committed step of extracting vanadium from stone coal in solution system.In industrial production, leachate adjusts acidity, reduction treatment
Afterwards, use acidic extractant P204 or P507 that organic phase is made for primary raw material to be extracted, rich vanadium liquid is obtained after back extraction.Extraction
During, it is primarily present problems with：(1) plurality of impurity ions can be extracted agent extraction, and foreign ion co-extraction influences vanadium extraction
Efficiency is taken, while contains more impurity in rich vanadium liquid, influences vanadium product purity；(2) acidic extractant P204 or P507 extracting golds
Belong to ion and belong to cation exchange mechanism, H is produced in extraction process+, decline pH value of solution, the optimal model of pH when deviateing vanadium extraction
Enclose, reduce vanadium extraction efficiency, extraction series increases.(3) phosphorus enters organic phase to carry secretly or other means in solution, through back extraction
Enter rich vanadium liquid after enrichment, be unfavorable for post precipitation recycling vanadium.
" method of extracting vanadium from bone coal navajoite leachate "（CN 102560115 A）Patented technology, the technology pass through leaching
Go out the preparation of liquid, reduced iron (III) is iron (II), extraction and back extraction and etc. control iron be extracted.This method is only limitted to treat
The control of iron in treatment fluid, the influence that other impurity and pH reduce to vanadium extraction can not Effective Regulation." a kind of acidity vanadium leaches
Phosphorus removing method in liquid "（CN 104480308 A）Patented technology.The pH for the acid vanadium leachate that the technology phosphorus removing method is related to
It is worth for 2.5 ~ 4.0, is the addition direct dephosphorization of composite dephosphorizing agent, mistake after reaction solution is aged again afterwards in acid leaching liquid
Filter, obtains the vanadium leachate of dephosphorization.Though this method can remove the phosphorus solution that pH value is 2.5 ~ 4.0, extracting vanadium from stone coal pickle liquor pH
Value is usually 0 ~ 2, and the hydrolysis of part metals ion, causes vanadium to lose when pH value is more than 2, and can form colloidal material and hinder vanadium extraction
Process carries out, therefore adopting said method dephosphorization has greater limitations.
The content of the invention
It is contemplated that the defects of overcoming the prior art, it is therefore an objective to provide a kind of solution ph in extraction process it is stable,
Extract purification enrichment vanadium in short series, vanadium and plurality of impurity ions good separating effect and the few pickle liquor from bone coal of rich vanadium liquid impurity
Method.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.0 ~ 1.4, separation of solid and liquid, obtains neutralizer with
And slag；Iron powder or sodium sulfite are added into the neutralizer again, 20 ~ 30min is stirred under the conditions of 15 ~ 60 DEG C；Then add
Salt of weak acid adjusts pH value to 1.7 ~ 2.0, obtains extraction stoste.
The iron powder addition is 1.0 ~ 1.2 times that Fe (III) is reduced to the theoretical amount of iron powder needed for Fe (II), described
The addition of sodium sulfite is also 1.0 ~ 1.2 times that Fe (III) is reduced to the theoretical amount of sodium sulfite needed for Fe (II).
Step 2: extraction
By extractant: TBP: the volume ratio of sulfonated kerosene is for (0.1 ~ 0.3): (0.02 ~ 0.1): 1 dispensing, mixes, is made
Organic phase；The extraction stoste is pressed again: the volume ratio of the organic phase is (2 ~ 6): 13 ~ 5 grades of counter-current extraction, obtains loading organic
Phase.
The temperature of the counter-current extraction is 15 ~ 40 DEG C, and the single-stage extraction time in the counter-current extraction is 5 ~ 10 min.
Step 3: washing
The weak alkaline aqueous solution that secure ph is 8 ~ 10 is detergent, by the load organic phases: the body of the detergent
Product is than being 1: (0.5 ~ 2) dispensing, washing into cleaning solution phosphorus concentration is less than 0.5 mg/L, obtains washing back loading organic phase.
Step 4: back extraction
Dose volume concentration is 5 ~ 12% H2SO4Solution is back washing agent, by the washing back loading organic phase: the back extraction
The volume ratio of agent is (4 ~ 12): 13 ~ 10 grades of countercurrent reextraction, obtains rich vanadium liquid and lean organic phase；Returned after lean organic phase regeneration treatment
Return extraction.
The temperature of the countercurrent reextraction is 20 ~ 50 DEG C, and the single-stage Stripping times in the countercurrent reextraction are 5 ~ 30 min.
The main chemical compositions of the bone coal pickle liquor are：V is 1.2 ~ 3.5g/L；Al is 7 ~ 25g/L；Fe is 2 ~ 9g/L；K
For 2.5 ~ 6g/L；P is 0.3 ~ 1.5g/L.
The calcareous material is CaCO3, CaO and Ca (OH)2One or more of.
Cation in the salt of weak acid is Na+、K+One or more of.
Anion in the salt of weak acid is PO4 3-、HPO4 2-、C2O4 2-One or more of.
The extractant is one kind in P204, P507, N235.
The weak alkaline aqueous solution is one or more of sodium hydroxide and potassium hydroxide.
Due to using the above method, compared with prior art, the present invention having the positive effect that：
1st, the method that the present invention uses adjusted stepwise pH value, the pH value of bone coal leachate is first adjusted to 1.0 ~ 1.4, reduce
Separation of solid and liquid load and vanadium loss；Salt of weak acid adjusting pH value to vanadium is added into neutralizer again and extracts optimum range 1.7 ~ 2.0,
Make to form weak acid root-weak acid buffer system in solution, to the H produced in extraction process+Into row buffering, raffinate pH stable
1.60 ~ 1.85.Compared with the raffinate pH value of the prior art reduces by 0.7 ~ 1.0, this method raffinate only reduces by 0.10 ~
0.25, the self-regulation of extraction system pH value is realized with pH stable 1.60 ~ 1.85, promotes vanadium extract and separate, extraction series contracting
1 ~ 3 grade short, aluminium content is only 10 ~ 25% of aluminium content in the rich vanadium liquid that other methods obtain in the rich vanadium liquid that the present invention obtains, this
It is only 20 ~ 35% of iron content in the rich vanadium liquid that other methods obtain to invent iron content in obtained rich vanadium liquid.
2nd, since the present invention uses weak alkaline aqueous solution to wash in organic phase and carry secretly and with weak chemical bond knot as detergent
The phosphorus of conjunction, phosphorus content is only 10 ~ 20% of phosphorus content in the rich vanadium liquid that other methods obtain in the obtained rich vanadium liquid of the present invention.
Therefore, the present invention has the solution ph in extraction process is stable, extracts short series, vanadium and plurality of impurity ions to divide
The characteristics of and richness vanadium liquid impurity good from effect is few.
Embodiment
With reference to embodiment, the invention will be further described, not to the limitation of its protection domain.
In present embodiment：
Cation in the salt of weak acid is Na+、K+One or more of；
Anion in the salt of weak acid is PO4 3-、HPO4 2-、C2O4 2-One or more of.
Repeated no more in embodiment.
Embodiment 1
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.The method comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.0 ~ 1.2, separation of solid and liquid, obtains neutralizer with
And slag；Iron powder is added into the neutralizer again, the addition of iron powder is that Fe (III) is reduced to the reason of iron powder needed for Fe (II)
1.0 ~ 1.1 times of stoichiometric；25 ~ 30min is stirred under the conditions of 15 ~ 30 DEG C, then addition salt of weak acid adjusting pH value to 1.7 ~ 1.9,
Obtain extraction stoste.
Step 2: extraction
By extractant: TBP: the volume ratio of sulfonated kerosene is for (0.1 ~ 0.2): (0.06 ~ 0.1): 1 dispensing, mixes, is made
Organic phase；The extraction stoste is pressed again: the volume ratio of the organic phase is (4 ~ 6): 13 ~ 4 grades of counter-current extraction, obtains loading organic
Phase.
The temperature of the counter-current extraction is 15 ~ 25 DEG C, and the single-stage extraction time in the counter-current extraction is 5 ~ 8 min.
Step 3: washing
The weak alkaline aqueous solution that secure ph is 8 ~ 9 is detergent, by the load organic phases: the volume of the detergent
Than for 1: (0.5 ~ 1) dispensing, washs into cleaning solution phosphorus concentration and be less than 0.5mg/L, washing back loading organic phase is obtained.
Step 4: back extraction
Dose volume concentration is 5 ~ 8% H2SO4Solution is back washing agent, by the washing back loading organic phase: the back extraction
The volume ratio of agent is (4 ~ 8): 13 ~ 6 grades of countercurrent reextraction, obtains rich vanadium liquid and lean organic phase；Returned after lean organic phase regeneration treatment
Extraction.
The temperature of the countercurrent reextraction is 20 ~ 30 DEG C, and the single-stage Stripping times in the countercurrent reextraction are 20 ~ 30 min.
The main chemical compositions of the bone coal pickle liquor are：V is 1.2 ~ 2.4g/L；Al is 7 ~ 14g/L；Fe is 6 ~ 9g/L；K
For 2.5 ~ 4.5g/L；P is 0.3 ~ 0.7g/L.
The calcareous material is CaCO3；The extractant is P204；The weak alkaline aqueous solution is sodium hydroxide.
Embodiment 2
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.The method comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.0 ~ 1.2, separation of solid and liquid, obtains neutralizer with
And slag；Sodium sulfite is added into the neutralizer again, the addition of sodium sulfite is that Fe (III) is reduced to needed for Fe (II)
1.0 ~ 1.1 times of the theoretical amount of sodium sulfite；25 ~ 30min is stirred under the conditions of 15 ~ 30 DEG C, salt of weak acid is then added and adjusts pH
Value obtains extraction stoste to 1.7 ~ 1.9.
Remaining is the same as embodiment 1.
Embodiment 3
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaCO except the calcareous material3Outside the mixture of CaO, remaining is the same as embodiment 1.
Embodiment 4
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaCO except the calcareous material3Outside the mixture of CaO, remaining is the same as embodiment 2.
Embodiment 5
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaCO except the calcareous material3, CaO and Ca (OH)2Mixture outside, remaining is the same as embodiment 1.
Embodiment 6
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaCO except the calcareous material3, CaO and Ca (OH)2Mixture outside, remaining is the same as embodiment 2.
Embodiment 7
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.The method comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.1 ~ 1.3, separation of solid and liquid, obtains neutralizer with
And slag；Iron powder is added into the neutralizer again, the addition of iron powder is that Fe (III) is reduced to the reason of iron powder needed for Fe (II)
1.05 ~ 1.15 times of stoichiometric；22 ~ 28min is stirred under the conditions of 30 ~ 45 DEG C, then add salt of weak acid adjust pH value to 1.7 ~
1.9, obtain extraction stoste.
Step 2: extraction
By extractant: TBP: the volume ratio of sulfonated kerosene is for (0.15 ~ 0.25): (0.04 ~ 0.08): 1 dispensing, mixing,
Organic phase is made；The extraction stoste is pressed again: the volume ratio of the organic phase is (2 ~ 4): 14 ~ 5 grades of counter-current extraction, is loaded with
Machine phase.
The temperature of the counter-current extraction is 20 ~ 35 DEG C, and the single-stage extraction time in the counter-current extraction is 6 ~ 9 min.
Step 3: washing
The weak alkaline aqueous solution that secure ph is 9 ~ 10 is detergent, by the load organic phases: the body of the detergent
Product is than being 1: (1.5 ~ 2) dispensing, washing into cleaning solution phosphorus concentration is less than 0.5mg/L, obtains washing back loading organic phase.
Step 4: back extraction
Dose volume concentration is 7 ~ 10% H2SO4Solution is back washing agent, by the washing back loading organic phase: the back extraction
The volume ratio of agent is (6 ~ 10): 17 ~ 10 grades of countercurrent reextraction, obtains rich vanadium liquid and lean organic phase；Returned after lean organic phase regeneration treatment
Return extraction.
The temperature of the countercurrent reextraction is 30 ~ 40 DEG C, and the single-stage Stripping times in the countercurrent reextraction are 15 ~ 25 min.
The main chemical compositions of the bone coal pickle liquor are：V is 2.4 ~ 3.5g/L；Al is 17 ~ 25g/L；Fe is 4 ~ 7g/L；
K is 4.5 ~ 6g/L；P is 1.0 ~ 1.5g/L.
The calcareous material is CaO；The extractant is P507；The weak alkaline aqueous solution is potassium hydroxide.
Embodiment 8
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.The method comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.1 ~ 1.3, separation of solid and liquid, obtains neutralizer with
And slag；Sodium sulfite is added into the neutralizer again, the addition of sodium sulfite is that Fe (III) is reduced to needed for Fe (II)
1.05 ~ 1.15 times of the theoretical amount of sodium sulfite；22 ~ 28min is stirred under the conditions of 30 ~ 45 DEG C, salt of weak acid is then added and adjusts
PH value obtains extraction stoste to 1.7 ~ 1.9.
Remaining is the same as embodiment 7.
Embodiment 9
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaO and Ca (OH) except the calcareous material2Mixture outside, remaining is the same as embodiment 7.
Embodiment 10
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaO and Ca (OH) except the calcareous material2Mixture outside, remaining is the same as embodiment 8.
Embodiment 11
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.The method comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.2 ~ 1.4, separation of solid and liquid, obtains neutralizer with
And slag；Iron powder is added into the neutralizer again, the addition of iron powder is that Fe (III) is reduced to the reason of iron powder needed for Fe (II)
1.1 ~ 1.2 times of stoichiometric；20 ~ 25min is stirred under the conditions of 45 ~ 60 DEG C, then addition salt of weak acid adjusting pH value to 1.8 ~ 2.0,
Obtain extraction stoste.
Step 2: extraction
By extractant: TBP: the volume ratio of sulfonated kerosene is for (0.25 ~ 0.3): (0.02 ~ 0.06): 1 dispensing, mixes, system
Obtain organic phase；The extraction stoste is pressed again: the volume ratio of the organic phase is (3 ~ 5): 14 ~ 5 grades of counter-current extraction, obtains loading organic
Phase.
The temperature of the counter-current extraction is 25 ~ 40 DEG C, and the single-stage extraction time in the counter-current extraction is 7 ~ 10 min.
Step 3: washing
The weak alkaline aqueous solution that secure ph is 9 ~ 10 is detergent, by the load organic phases: the body of the detergent
Product is than being 1: (1 ~ 1.5) dispensing, washing into cleaning solution phosphorus concentration is less than 0.5mg/L, obtains washing back loading organic phase.
Step 4: back extraction
Dose volume concentration is 9 ~ 12% H2SO4Solution is back washing agent, by the washing back loading organic phase: the back extraction
The volume ratio of agent is (8 ~ 12): 15 ~ 8 grades of countercurrent reextraction, obtains rich vanadium liquid and lean organic phase；Returned after lean organic phase regeneration treatment
Extraction.
The temperature of the countercurrent reextraction is 40 ~ 50 DEG C, and the single-stage Stripping times in the countercurrent reextraction are 5 ~ 15 min.
The main chemical compositions of the bone coal pickle liquor are：V is 1.8 ~ 3.0g/L；Al is 10 ~ 18g/L；Fe is 2 ~ 5g/L；
K is 3.5 ~ 5g/L；P is 0.6 ~ 1.1g/L.
The calcareous material is Ca (OH)2；The extractant is N235；The weak alkaline aqueous solution is sodium hydroxide
With the mixture of potassium hydroxide.
Embodiment 12
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.The method comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.2 ~ 1.4, separation of solid and liquid, obtains neutralizer with
And slag；Sodium sulfite is added into the neutralizer again, the addition of sodium sulfite is that Fe (III) is reduced to needed for Fe (II)
1.1 ~ 1.2 times of the theoretical amount of sodium sulfite；20 ~ 25min is stirred under the conditions of 45 ~ 60 DEG C, salt of weak acid is then added and adjusts pH
Value obtains extraction stoste to 1.8 ~ 2.0.
Remaining is the same as embodiment 11.
Embodiment 13
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaCO except the calcareous material3With Ca (OH)2Mixture outside, remaining is the same as embodiment 11.
Embodiment 14
A kind of method of purification enrichment vanadium in pickle liquor from bone coal.
The present embodiment is CaCO except the calcareous material3With Ca (OH)2Mixture outside, remaining is the same as embodiment 12.
Present embodiment compared with prior art, has the positive effect that：
1st, the method that present embodiment uses adjusted stepwise pH value, first adjust the pH value of bone coal leachate to 1.0 ~
1.4, reduce separation of solid and liquid load and vanadium loss；Salt of weak acid is added into neutralizer again and adjusts pH value to vanadium extraction optimum range
1.7 ~ 2.0, make to form weak acid root-weak acid buffer system in solution, to the H produced in extraction process+Into row buffering, raffinate
PH stable is 1.60 ~ 1.85.Compared with the raffinate pH value of the prior art reduces by 0.7 ~ 1.0, this method raffinate only reduces
0.10 ~ 0.25, the self-regulation of extraction system pH value is realized with pH stable 1.60 ~ 1.85, is promoted vanadium extract and separate, is extracted level
Number shortens 1 ~ 3 grade, in the rich vanadium liquid that present embodiment obtains aluminium content be only in the rich vanadium liquid that other methods obtain aluminium contain
The 10 ~ 25% of amount, iron content is only iron content in the rich vanadium liquid that other methods obtain in the rich vanadium liquid that present embodiment obtains
20 ~ 35%.
2nd, since present embodiment uses weak alkaline aqueous solution to wash in organic phase and carry secretly and with weak as detergent
The phosphorus of chemical bonds, phosphorus content is only phosphorus in the rich vanadium liquid that other methods obtain in the rich vanadium liquid that present embodiment obtains
The 10 ~ 20% of content.
Therefore, present embodiment have the solution ph in extraction process is stable, extraction series is short, vanadium with it is a variety of miscellaneous
The characteristics of good and rich vanadium liquid impurity of matter ion isolation effect is few.
Claims (6)
1. a kind of method of purification enrichment vanadium in pickle liquor from bone coal, it is characterised in that the method comprises the concrete steps that：
Step 1: prepared by extraction stoste
Calcareous material is added in bone coal pickle liquor, adjusts pH value to 1.0~1.4, separation of solid and liquid, obtains neutralizer with neutralizing
Slag；Iron powder or sodium sulfite are added into the neutralizer again, 20~30min is stirred under the conditions of 15~60 DEG C；Then add
Salt of weak acid adjusts pH value to 1.7~2.0, obtains extraction stoste；
The iron powder addition is 1.0~1.2 times that Fe (III) is reduced to the theoretical amount of iron powder needed for Fe (II), the Asia
The addition of sodium sulphate is also 1.0~1.2 times that Fe (III) is reduced to the theoretical amount of sodium sulfite needed for Fe (II)；
Step 2: extraction
By extractant: TBP: the volume ratio of sulfonated kerosene is (0.1~0.3): (0.02~0.1): 1 dispensing, mixing, is made organic
Phase；The extraction stoste is pressed again: the volume ratio of the organic phase is (2~6): 1 3~5 grades of counter-current extraction, obtains load organic phases；
The temperature of the counter-current extraction is 15~40 DEG C, and the single-stage extraction time in the counter-current extraction is 5~10min；
Step 3: washing
The weak alkaline aqueous solution that secure ph is 8~10 is detergent, by the load organic phases: the volume ratio of the detergent
For 1: (0.5~2) dispensing, washs into cleaning solution phosphorus concentration and be less than 0.5mg/L, washing back loading organic phase is obtained；
Step 4: back extraction
Dose volume concentration is 5~12% H2SO4Solution is back washing agent, by the washing back loading organic phase: the back washing agent
Volume ratio be (4~12): 1 3~10 grades of countercurrent reextraction, obtains rich vanadium liquid and lean organic phase；Returned after lean organic phase regeneration treatment
Return extraction；
The temperature of the countercurrent reextraction is 20~50 DEG C, and the single-stage Stripping times in the countercurrent reextraction are 5~30min；
Anion in the salt of weak acid is PO4 3-、HPO4 2-、C2O4 2-One or more of.
2. the method for purification enrichment vanadium in the pickle liquor according to claim 1 from bone coal, it is characterised in that the bone coal acid
The main chemical compositions of immersion liquid are：V is 1.2~3.5g/L；Al is 7~25g/L；Fe is 2~9g/L；K is 2.5~6g/L；P is
0.3~1.5g/L.
3. the method for purification enrichment vanadium in the pickle liquor according to claim 1 from bone coal, it is characterised in that the calcic thing
Matter is CaCO3, CaO and Ca (OH)2One or more of.
4. the method for purification enrichment vanadium in the pickle liquor according to claim 1 from bone coal, it is characterised in that the salt of weak acid
In cation be Na+、K+One or more of.
5. the method for purification enrichment vanadium in the pickle liquor according to claim 1 from bone coal, it is characterised in that the extractant
For one kind in P204, P507 and N235.
6. the method for purification enrichment vanadium in the pickle liquor according to claim 1 from bone coal, it is characterised in that the alkalescent
Aqueous solution is one or more of sodium hydroxide and potassium hydroxide.
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