CN108754187A - A method of with microemulsion from solution Selective Separation vanadium phosphorus - Google Patents

A method of with microemulsion from solution Selective Separation vanadium phosphorus Download PDF

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Publication number
CN108754187A
CN108754187A CN201810788188.9A CN201810788188A CN108754187A CN 108754187 A CN108754187 A CN 108754187A CN 201810788188 A CN201810788188 A CN 201810788188A CN 108754187 A CN108754187 A CN 108754187A
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solution
vanadium
phosphorus
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concentration
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李鸿乂
郭赟
林敏敏
杨阳
谢兵
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Chongqing University
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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
    • 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
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The method of the invention discloses a kind of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and the solution A that phosphorus containing vanadium is 1g/L is obtained after stirring；It is to be adjusted to 3.0~8.3 by the pH value of solution A；2) methyl tricapryl ammonium chloride and isoamyl alcohol are added in normal heptane, mixture A is obtained after stirring；3) mixed solution containing NaOH and NaCl is added dropwise into mixture A, is stood after being stirred until homogeneous, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains mixture B；5) mixture B is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；6) concentration of organic phase vanadium and phosphorus is calculated with material balance method realizes the highly selective separation of vanadium phosphorus to calculate vanadium phosphorus extraction yield and vanadium phosphorus separation.

Description

A method of with microemulsion from solution Selective Separation vanadium phosphorus
Technical field
The present invention relates to Selective Separation vanadium phosphorus fields, more particularly to a kind of to use microemulsion Selective Separation vanadium from solution The method of phosphorus.
Background technology
Vanadium is important strategic resource, is widely used in the industries such as steel, national defence, automobile, aerospace.For navajoite resource Extensive exploitation using creating condition.Current main extraction vanadium method is Leaching of Vanadium from Vanadium slag, and Leaching of Vanadium from Vanadium slag method is generally exactly at present By vanadium slag by roasting, leaching, it is then further processed precipitation, finally obtains this method of vanadium product.
What this method obtained has a large amount of impurity containing vanadium leachate, and difficulty is increased to cleaning procedure.Especially phosphorus Presence great harm can be brought to post-processing, especially very big to the influence of precipitation, phosphorus and vanadium can form stable complexing Object H7[P(V2O5)6], it can also be with Fe3+、Al3+Calcium phosphate precipitation is generated, APV is polluted, influences the quality of vanadic anhydride.
For vanadium-bearing slag of high calcium and high phosphor, the concentration of phosphorus is higher in the leachate finally obtained, at present containing dephosphorization in vanadium leachate Method dephosphorization agent is mainly added, dephosphorization agent and phosphorus reaction, which generate, to be precipitated, then is separated by solid-liquid separation, and the leaching of the vanadium after dephosphorization is obtained Go out liquid；The impurity in the vanadium leachate after dephosphorization is removed again, obtains vanadium leachate.
But this technique has the following defects：
1) phosphorus content of the vanadium leachate obtained is very high, and the dosage of vanadium leachate dephosphorization agent during dephosphorization is very big, Cause dephosphorization of high cost.
2) still very high by the remaining phosphorus content in the vanadium leachate after dephosphorization agent dephosphorization, it is unable to get low-phosphorous Vanadium leachate；
3) it also needs to be separated by solid-liquid separation dephosphorization agent after the technique dephosphorization, is separated by solid-liquid separation operation and carries out removal of impurities behaviour later Make so that entire process for extracting vanadium process is more complicated, and the use equipment in vanadium extracting process is increased, and causes from high calcium height Vanadium extraction cost in phosphorus vanadium slag is very high；
4) during vanadium leachate practical dephosphorization, dephosphorization agent and phosphorus reaction generate while precipitate, and part vanadium also can be with Dephosphorization agent reaction generates precipitation, leads to the loss that vanadium is caused during dephosphorization.
Therefore, need in the prior art it is a kind of with microemulsion from solution Selective Separation vanadium phosphorus method.
Invention content
Present invention aim to address problems of the prior art, provide a kind of selective from solution with microemulsion The method for detaching vanadium phosphorus.
To realize the present invention purpose and the technical solution adopted is that such, it is a kind of selectively to be divided from solution with microemulsion Method from vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and the solution that phosphorus containing vanadium is 1g/L is obtained after stirring A；
It is to be adjusted to 3.0~8.3 by the pH value of solution A；
2) surfactant/extractant, cosurfactant are added in dispersant, mixture A is obtained after stirring；
Surfactant/the extractant is methyl tricapryl ammonium chloride；The weight of the methyl tricapryl ammonium chloride accounts for The 2%~30% of mixture A total amounts；
The one kind of the cosurfactant in isoamyl alcohol, n-butanol, n-hexyl alcohol, n-heptanol or n-octyl alcohol；It is described The weight of cosurfactant accounts for the 10%~30% of mixture A total amounts；
The one kind of the dispersant in normal heptane or sulfonated kerosene；
3) mixed solution containing NaOH and NaCl is added dropwise in the mixture A obtained into step 2), after being stirred until homogeneous It stands, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.1~1.0mol/L of NaOH solution, NaCl solution a concentration of 0.1~ 1.0mol/L；
Volume ratio (10~5) ︰ 1 of the mixture A and mixed solution；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ (1~30)；
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient.
Further, the process of the adjusting pH value of the step 1) is：H is added into solution A2SO4And NaOH.
Further, in the whipping process in the step 3)：Speed of agitator is 200r/min, mixing time 5min.
Further, in the whipping process in the step 4)：Stir speed (S.S.) be 100~200r/min, mixing time be 1~ 5min。
The solution have the advantages that unquestionable, the present invention has the following advantages：
1) extractant that the present invention selects has the selectivity of height, and phosphate radical is much larger than to the affinity of vanadic acid root, this It is the basis for realizing Selective Separation vanadium, phosphorus；
2) present invention improves mass transfer velocity using microemulsion as the carrier of extractant due to microemulsion large specific surface area, Reduce the reaction time；
3) microemulsion in the present invention prepares simple, and extraction process and traditional extraction are essentially identical, technology maturation, and Single-stage extraction can do the trick；
4) this method step is simple, easy to operate.
In conclusion the present invention provides a kind of with the highly selective separation vanadium phosphorus of microemulsion, recycling containing in vanadium, phosphorus solution The method of v element.
Specific implementation mode
With reference to embodiment, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention only It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used With means, various replacements and change are made, should all include within the scope of the present invention.
Embodiment 1：
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 3.0 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and isoamyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the isoamyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The w/v of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.67%, and the extraction yield of phosphorus is 7.47%, and vanadium phosphorus separation is 3794.
Embodiment 2：
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 4.0 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and isoamyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the isoamyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.87%, and the extraction yield of phosphorus is 5.38%, and vanadium phosphorus separation is 13126.
Embodiment 3：
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and isoamyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the isoamyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.83%, and the extraction yield of phosphorus is 2.75%, and vanadium phosphorus separation is 20180.
Embodiment 4
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and n-butanol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the n-butanol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.87%, and the extraction yield of phosphorus is 2.83%, and vanadium phosphorus separation is 25392.
Embodiment 5
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and n-hexyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the n-hexyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.75%, and the extraction yield of phosphorus is 1.97%, and vanadium phosphorus separation is 33848.
Embodiment 6
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and n-heptanol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the n-heptanol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.67%, and the extraction yield of phosphorus is 2.76%, and vanadium phosphorus separation is 27445.
Embodiment 7
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and n-octyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the n-octyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.85%, and the extraction yield of phosphorus is 5.01%, and vanadium phosphorus separation is 12081.
Embodiment 8
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) mixture A is obtained after methyl tricapryl ammonium chloride and isoamyl alcohol being added to sulfonated kerosene stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the isoamyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.5mol/L of NaOH solution, a concentration of 0.5mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.64%, and the extraction yield of phosphorus is 3.56%, and vanadium phosphorus separation is 20570.
Embodiment 9
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and isoamyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the isoamyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.7mol/L of NaOH solution, a concentration of 0.7mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.73%, and the extraction yield of phosphorus is 4.15%, and vanadium phosphorus separation is 15766.
Embodiment 10
A method of with microemulsion from solution Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and isoamyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the isoamyl alcohol accounts for the 20% of mixture A total amounts；
3) mixed solution containing NaOH and NaCl is slowly added dropwise in the mixture A obtained into step 2), stirs to equal It is stood after even, split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.3mol/L of NaOH solution, a concentration of 0.3mol/L of NaCl solution；
The volume ratio of the mixture A and mixed solution is 5:1；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, obtains To mixture B；
The volume ratio of the microemulsion and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.81%, and the extraction yield of phosphorus is 4.65%, and vanadium phosphorus separation is 12597.
Comparative example 1:
The method of general solvent extraction Selective Separation vanadium phosphorus, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and it is 1g/L that 1000mL phosphorus containing vanadium is obtained after stirring Solution A；
It is to be adjusted to 5.2 by the pH value of solution A；
Adjust pH value process be：H is added into solution A2SO4And NaOH.
2) methyl tricapryl ammonium chloride and isoamyl alcohol are added in normal heptane, mixture A is obtained after stirring；
The 14% of the weight mixture A total amounts of the methyl tricapryl ammonium chloride；
The weight of the isoamyl alcohol accounts for the 20% of mixture A total amounts；
3) it by the solution A of the phosphorus containing vanadium obtained in the mixture A and step 1) that are obtained in step 2), is stirred, obtains Mixture B；
The volume ratio of the mixture A and solution A is 1 ︰ 4；
In the whipping process：Stir speed (S.S.) is 200r/min, and mixing time is 1~5min.
4) the mixture B obtained in step 3) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
5) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and the separation of vanadium phosphorus Coefficient；
It is computed, the extraction yield of vanadium is 99.68%, and the extraction yield of phosphorus is 5.75%, and vanadium phosphorus separation is 9187.

Claims (4)

1. it is a kind of with microemulsion from solution Selective Separation vanadium phosphorus method, which is characterized in that include the following steps：
1) by Na3VO4·12H2O and Na3PO4·12H2O is added to the water, and the solution A that phosphorus containing vanadium is 1g/L is obtained after stirring；
It is to be adjusted to 3.0~8.3 by the pH value of solution A；
2) surfactant/extractant, cosurfactant are added in dispersant, mixture A is obtained after stirring；
Surfactant/the extractant is methyl tricapryl ammonium chloride；The weight of the methyl tricapryl ammonium chloride accounts for mixing The 2%~30% of object A total amounts；
The one kind of the cosurfactant in isoamyl alcohol, n-butanol, n-hexyl alcohol, n-heptanol or n-octyl alcohol；It is described to help table The weight of face activating agent accounts for the 10%~30% of mixture A total amounts；
The one kind of the dispersant in normal heptane or sulfonated kerosene；
3) mixed solution containing NaOH and NaCl is added dropwise in the mixture A obtained into step 2), is stood after being stirred until homogeneous, Split-phase is carried out after clarification, upper phase is the W/O microemulsions of saturation；
In the mixed solution, a concentration of 0.1~1.0mol/L of NaOH solution, a concentration of 0.1~1.0mol/ of NaCl solution L；
Volume ratio (10~5) ︰ 1 of the mixture A and mixed solution；
4) it by the solution A of the phosphorus containing vanadium obtained in the W/O microemulsions and step 1) that are obtained in step 3), is stirred, is mixed Close object B.
The volume ratio of the microemulsion and solution A is 1 ︰ (1~30)；
5) the mixture B obtained in step 4) is subjected to stratification, takes out lower layer's water phase, detect the concentration of vanadium phosphorus；
6) concentration that organic phase vanadium and phosphorus are calculated with material balance method, to calculate vanadium phosphorus extraction yield and vanadium phosphorus segregative line Number.
2. it is according to claim 1 or 2 it is a kind of with microemulsion from solution Selective Separation vanadium phosphorus method, feature exists In：The process of the adjusting pH value of the step 1) is：H is added into solution A2SO4And NaOH.
3. it is according to claim 1 or 2 it is a kind of with microemulsion from solution Selective Separation vanadium phosphorus method, feature exists In：In whipping process in the step 3)：Speed of agitator is 200r/min, mixing time 5min.
4. it is according to claim 1 it is a kind of with microemulsion from solution Selective Separation vanadium phosphorus method, it is characterised in that： In whipping process in the step 4)：Stir speed (S.S.) is 100~200r/min, and mixing time is 1~5min.
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