CN107604162A - A kind of mixed extractant for separating yttrium - Google Patents
A kind of mixed extractant for separating yttrium Download PDFInfo
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- CN107604162A CN107604162A CN201710817817.1A CN201710817817A CN107604162A CN 107604162 A CN107604162 A CN 107604162A CN 201710817817 A CN201710817817 A CN 201710817817A CN 107604162 A CN107604162 A CN 107604162A
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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
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- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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Abstract
The invention discloses a kind of mixed extractant for separating yttrium, the mixed extractant press volume percentage consisting of：Aphthenic acids 10~60%, basic extractant 10~50%, alcohols material 5~40%, diluent 10~60%.Mixed extractant of the present invention is less demanding to the acid number of aphthenic acids, during using the mixed extractant separating yttrium, without carrying out saponification process to the mixed extractant containing aphthenic acids, the content of yttrium in rare earth feed liquid is not required, aphthenic acids will not be dissolved in aqueous phase and realize free of losses in extraction process, compared to the concentration that saponification cycloalkanes acid system can effectively reduce back extraction acid.
Description
The application be " be used for separating yttrium mixed extractant and from rare earth feed liquid extract and separate yttrium method " division
Application, the applying date of original application is：On December 24th, 2015, Application No.：It is 201510982402.0 entitled：For
The mixed extractant of separating yttrium and from rare earth feed liquid extract and separate yttrium method.
Technical field
The present invention relates to the isolation technics of yttrium, and in particular to a kind of mixed extractant for separating yttrium and from rare earth feed liquid
The method of middle extract and separate yttrium.
Background technology
Yttrium (Y) is a kind of important rare earth element, is widely used in Aero-Space, luminescent material, nuclear energy and metallurgical industry
Field, and purity requirement of these fields to yttrium is all higher.Yttrium is primarily present in Rare Earth Mine, from rare earth feed liquid (Rare Earth Mine
Pickle liquor) in extraction yttrium be obtain high-purity yttrium main path.Generally use solvent extraction is from the rare earth feed liquid containing yttrium
Separating yttrium, most widely used extractant are aphthenic acids.
Aphthenic acids belongs to acidic extractant, needs to carry out saponification process using ammoniacal liquor before yttrium is extracted, this results in saponification
Step and follow-up yttrium extraction step produce substantial amounts of ammonia nitrogen waste water, are directly discharged if this effluent part is untreated, it will
Serious environmental pollution is caused, and needs to increase sewage-treatment plant if waste water is handled, is thrown so as to greatly increase equipment
Money and production cost.
Aphthenic acids is the mixture of carboxylic acids containing different carbon numbers, while also have containing other from oil refining product
The material such as machine acid (aliphatic acid and aromatic carboxylic acid), inorganic acid, neutral oil, oil phenols and mercaptan, thus needed before use pair
Aphthenic acids is refined, and to be separated off the compositions such as aliphatic acids, cyclohexylenedinitrilotetraacetic acid, phenols and neutral oil therein, then is used
The methods of distillation, obtains the aphthenic acids of different fractions.The aphthenic acids of distillation gained different fractions has different carbon number and acid
Value, the aphthenic acids of usual high acid value are higher to the extraction yield of yttrium.Therefore, yttrium extraction aphthenic acids used is after refined mostly
High acid value aphthenic acids, such as to the cycloalkanes in the aphthenic acids and Karamay Region, Xinjiang oil in the oil of China Bay areas
Acid be evaporated under reduced pressure obtained by cut in, wherein the acid number of 120~200 DEG C of cut is higher than 180mg/g mostly, less than 120
DEG C and be respectively lower than 100mgKOH/g and 180mgKOH/g higher than the acid number of 200 DEG C of cuts, and these acid numbers are less than 180mgKOH/
G cut is all relatively low to the extraction yield of yttrium, be not suitable for yttrium extractant (rare element specialty aphthenic acids group aphthenic acids and
Its property of research (I)-some aphthenic acids and the selection Fudan Journal (natural sciences of extractant to rare earth element extraction
Version), 1977, (4)：73-82,110).Because the composition of the naphthenic acid raw material of different manufacturers offer is not quite similar, cause aphthenic acids
, it is necessary to often adjust naphthenic acid raw material process for refining condition and the process conditions of yttrium extraction, this makes life during extractant as yttrium
Production operation becomes cumbersome.
Aphthenic acids has certain solubility in water, in the prior art, with always some ring after cycloalkanes acid extraction yttrium
Alkanoic acid enters in aqueous phase, and this not only causes the significant wastage of organic phase, and raffinate needs to enter after removing organic phase
Subsequent processing or discharge, while fresh aphthenic acids need to be continuously replenished in production process, which increases production cost.
In addition, saponification cycloalkanes acid system typically requires that yttrium content could extract yttrium higher than 65% in feed liquid in the prior art,
If yttrium content be less than 65%, it usually needs first carry out preenrichment (such as other rare earth compositions are separated) make yttrium content reach 65% with
Cycloalkanes acid system could be used to separate after upper.
The content of the invention
The technical problem to be solved in the present invention is to be directed to the deficiencies in the prior art, there is provided a kind of for separating yttrium
Mixed extractant and from rare earth feed liquid extract and separate yttrium method.Mixed extractant of the present invention, to the acid of aphthenic acids
Be worth it is less demanding, using mixed extractant of the present invention from rare earth feed liquid extract and separate yttrium when, yttrium in rare earth feed liquid is contained
Amount is not required, and aphthenic acids does not lose in extraction process.
Mixed extractant of the present invention for separating yttrium, by volume percentage, the composition of the mixed extractant
For：
Aphthenic acids 10~60%, basic extractant 10~50%, alcohols material 5~40%, diluent 10~60%.
The composition of above-mentioned mixed extractant is preferably by volume percentage：
Aphthenic acids 20~40%, basic extractant 15~40%, alcohols material 10~30%, diluent 20~40%.
In the technical scheme of above-mentioned mixed extractant, described aphthenic acids is the naphthenic acid raw material of producer's offer by existing normal
The refining step of rule removes the aphthenic acids of gained after the impurity such as neutral oil, aliphatic acid and phenols mercaptan therein.It is of the invention preferred
Use aphthenic acids of the acid number for 50~250mgKOH/g.
In the technical scheme of above-mentioned mixed extractant, described basic extractant can be trialkyl tertiary amine (N235) or secondary
Carbon primary amine (N1923).
In the technical scheme of above-mentioned mixed extractant, described alcohols material can be in the alcohol containing 2~8 carbon atoms
One or more kinds of combinations, can be specifically selected from ethanol, normal propyl alcohol, isopropanol, n-butanol, n-amyl alcohol, n-hexyl alcohol, just
Combination more than one or both of enanthol, sec-octyl alcohol, isooctanol.When the group that the selection of alcohols material is above-mentioned any two kinds
During conjunction, the proportioning between them can be any proportioning.
In the technical scheme of above-mentioned mixed extractant, described diluent is selected from kerosene, hexamethylene, n-hexane and positive heptan
Combination more than one or both of alkane.When the selection of diluent is above-mentioned any two kinds of combination, matching somebody with somebody between them
Than that can be any proportioning.
The present invention also provides a kind of method of the extract and separate yttrium from rare earth feed liquid, and this method uses above-mentioned mixed extractant
Extractant as the extract and separate yttrium from rare earth feed liquid.
The method of the extract and separate yttrium of the present invention from rare earth feed liquid, including the first fractional extraction process and second point
Extraction process is evaporated, rare earth feed liquid and above-mentioned mixed extractant are sent into the first fractional extraction process carries out extract and separate, respectively
To the feed liquid a containing Y and other difficult separation of rare earth elements, and the feed liquid b containing other easily separated rare earth elements；By feed liquid a and
Above-mentioned mixed extractant is sent into after-fractionating extraction process and carries out extract and separate, respectively obtains feed liquid d containing Y and containing other difficulties
The feed liquid c of separation of rare earth elements.
In the method for the above-mentioned extract and separate yttrium from rare earth feed liquid, the first described fractional extraction process and after-fractionating extraction
Process is taken to include three extraction, washing and back extraction workshop sections, wherein：
Extraction, washing and three workshop section's processing of back extraction of the first fractional extraction process are as follows：
In extraction section, using above-mentioned mixed extractant as organic phase, the 1st grade of extraction section is sent into, rare earth feed liquid is sent into and extracted
Take a section afterbody；The flow-rate ratio of the organic phase and feed liquid is 6~1:1；
In washing section, using the liquid that outflow is exported from extraction section afterbody as organic phase, washing section the 1st is sent directly into
Level；Using 0.1~1mol/L hydrochloric acid as cleaning solution, washing section afterbody is sent into；From the cleaning solution of washing section first order outflow
It is sent directly into extraction section afterbody；The organic phase and the flow-rate ratio of cleaning solution are 1:0.5~2；
In stripping section, using the liquid that outflow is exported from washing section afterbody as organic phase, stripping section the 1st is sent directly into
Level；Using 0.5~2.5mol/L hydrochloric acid solution as back extraction acid solution, stripping section afterbody is sent into；In stripping section, organic phase with
The flow-rate ratio for being stripped acid solution is 5~1:1~2；
After the first fractional extraction process, collected from the 1st grade of outlet of extraction section and contain Y and other difficult separation of rare earth elements
Raffinate be feed liquid a, it is feed liquid b to collect the strip liquor containing other easily separated rare earth elements from the outlet of the 1st grade of stripping section, from anti-
Extract the last 1 grade of outlet of section and collect blank organic phase (i.e. blank mixed extractant, similarly hereinafter), return to the extraction section first order and repeat to make
With；
Extraction, washing and three workshop section's processing of back extraction of the after-fractionating extraction process are as follows：
In extraction section, using above-mentioned mixed extractant as organic phase, the 1st grade of extraction section is sent into, feed liquid a is sent into extraction section
Afterbody；The organic phase and feed liquid a flow-rate ratio are 6~1:1；
In washing section, using the liquid that outflow is exported from extraction section afterbody as organic phase, washing section the 1st is sent directly into
Level；Using 0.1~1mol/L hydrochloric acid as cleaning solution, washing section afterbody is sent into；From the cleaning solution of washing section first order outflow
It is sent directly into extraction section afterbody；The organic phase and the flow-rate ratio of cleaning solution are 1:0.5~2；
In stripping section, using the liquid that outflow is exported from washing section afterbody as organic phase, stripping section the 1st is sent directly into
Level；Using 0.5~2.5mol/L hydrochloric acid solution as back extraction acid solution, stripping section afterbody is sent into；In stripping section, organic phase with
The flow-rate ratio for being stripped acid solution is 5~1:1~2；After after-fractionating extraction process, collected from the 1st grade of outlet of extraction section and contain it
The feed liquid c of its difficult separation of rare earth elements, the feed liquid d containing Y is collected from the 1st grade of outlet of stripping section, received from the last 1 grade of outlet of stripping section
Collect blank organic phase, return to the extraction section first order and reuse.
In the method for the extract and separate yttrium of the present invention from rare earth feed liquid, described rare earth feed liquid is the chlorination of Rare Earth Mine
Leachate, wherein contain Y, and also containing 14 kinds of rare earths such as La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu
Any one in element or two or more rare earth elements.Applicant has found during long-term experiment, works as rare earth feed liquid
During containing 15 kinds of rare earth elements such as La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y, of the present invention
Extraction system in, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu therein belong to easily separated element, La, Ce, Pr, Nd, Y
Belong to difficult separating element；When in rare earth feed liquid only containing 5 kinds of elements such as La, Ce, Pr, Nd, Y, La, Ce, Pr, Nd belong to difficult point
From element, Y belongs to easily separated element.Scheme of the present invention is not required to the content of Y in rare earth feed liquid, no matter Y contents are
Higher than 65% again below 65%, can technical scheme of the present invention be used to carry out extract and separate.
Compared with prior art, the method have the characteristics that：
1st, compared with the technology of traditional aphthenic acids extract and separate yttrium, the method for the invention can not only use high acid value ring
Alkanoic acid is extracted, and can also be extracted with low acid number aphthenic acids, so as to eliminate the distillation of naphthenic acid raw material processing to obtain
The step of obtaining high acid value aphthenic acids, not only increases the utilization rate of naphthenic acid raw material, is omitted further to naphthenic acid raw material
The step of distillation, reduce equipment investment expense and feed purification expense.
2nd, extraction separation process is not required to carry out saponification process to the mixed extractant containing aphthenic acids, eliminates ammonia soap step,
The processing and discharge of ammonia nitrogen waste water are avoided, the generation of environmental pollution is avoided from source.
3rd, the concentration of the back extraction acid of saponification cycloalkanes acid system is typically in more than 3mol/L, and present invention back extraction acid used is dense
Degree is less than 3mol/L, and the method for the invention significantly reduces the sour dosage of back extraction；Spent acid content in blank organic phase after back extraction
It is very low, it is not required to carry out to wash acid operation and can return to extraction section and recycle, eliminates organic phase and wash the water consumption that acid operates.
4th, because mixed extractant uses special composition and ratio, make that in extraction process aphthenic acids aqueous phase will not be dissolved in
In, it is entirely avoided the loss of organic phase, cycling extraction process are not required to supplement fresh aphthenic acids, save extractant consumption.
5th, yttrium is extracted using cycloalkanes acid system of the present invention, there is no concentration limitation, nothing to the yttrium content in rare earth feed liquid
65% is above again below 65% by yttrium content, can use mixed extractant of the present invention to carry out extract and separate.
6th, extract and separate is carried out to the yttrium in rare earth feed liquid using mixed extractant of the present invention, operation is simple,
Method cost is low, has significant economic benefit.
Brief description of the drawings
Fig. 1 is the process chart of the embodiment of the present invention 1, and wherein n represents extraction section afterbody, and m represents washing section most
Rear stage, p represent stripping section afterbody.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, to more fully understand present disclosure, but
The present invention is not limited to following examples.
Embodiment 1：Mixed extractant
By percent by volume, measure 25% aphthenic acids (acid number 150mgKOH/g), 30% N235,20% it is different pungent
Alcohol and 25% kerosene, it is well mixed, obtains mixed extractant.
Embodiment 2：Mixed extractant
By percent by volume, 20% aphthenic acids (acid number 120mgKOH/g), 50% N235,20% Zhong Xin are measured
Alcohol and 10% normal hexane, it is well mixed, obtains mixed extractant.
Embodiment 3：Mixed extractant
By percent by volume, measure 10% aphthenic acids (acid number 180mgKOH/g), 20% N235,40% it is different pungent
Alcohol, 15% kerosene and 15% hexamethylene, it is well mixed, obtains mixed extractant.
Embodiment 4：Mixed extractant
By percent by volume, measure 15% aphthenic acids (acid number 150mgKOH/g), 20% N235, positive the penta of 30%
Alcohol and 35% hexamethylene, it is well mixed, obtains mixed extractant.
Embodiment 5：Mixed extractant
By percent by volume, 30% aphthenic acids (acid number 150mgKOH/g), 10% N1923,15% just are measured
Hexanol and 45% normal heptane, it is well mixed, obtains mixed extractant.
Embodiment 6：Mixed extractant
By percent by volume, 20% aphthenic acids (acid number 80mgKOH/g), 40% N235,15% positive fourth are measured
Alcohol and 25% kerosene, it is well mixed, obtains mixed extractant.
Embodiment 7：Mixed extractant
By percent by volume, measure 30% aphthenic acids (acid number 150mgKOH/g), 25% N1923,35% it is different
Propyl alcohol and 10% hexamethylene, it is well mixed, obtains mixed extractant.
Embodiment 8：Mixed extractant
By percent by volume, 60% aphthenic acids (acid number 50mgKOH/g), 15% N1923,5% ethanol are measured
Normal heptane with 20%, is well mixed, obtains mixed extractant.
Embodiment 9：Mixed extractant
By percent by volume, measure 10% aphthenic acids (acid number 50mgKOH/g), 10% N1923, positive the third of 20%
Alcohol, 20% hexamethylene, 20% n-hexane and 20% sulfonated kerosene, it is well mixed, obtains mixed extractant.
Embodiment 10：Using the method for mixed extractant extract and separate yttrium from rare earth feed liquid
La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y concentration are 42.2g/L in rare earth feed liquid,
10.5g/L,10.7g/L,39.4g/L,8.3g/L,1.6g/L,9.7g/L,1.8g/L,8.4g/L,1.7g/L,4.7g/L,
0.4g/L,4.1g/L,0.5g/L,42.7g/L。
In the first fractional extraction process, mixed extractant made from embodiment 1 is added to the 1st grade of extraction section, will be dilute
Earth material liquid is added to last 1 grade of extraction section, using 1mol/L hydrochloric acid solutions as cleaning solution, is added to last 1 grade of washing section；Mixing
Extractant, rare earth feed liquid, the flow-rate ratio of cleaning solution are 4：1：1.5.By 13 grades of extractions, 10 grades of washings, in extraction section, the 1st grade goes out
Mouth obtains the feed liquid (being represented with feed liquid a) containing La, Ce, Pr, Nd, Y, yield 99%；With the liquid of the last 1 grade of outflow of washing section
For organic phase, the 1st grade of stripping section is sent into, using 2.5mol/L hydrochloric acid solution as back extraction acid solution, last 1 grade of stripping section is sent into, has
The flow-rate ratio of machine phase and back extraction acid solution is 3:1, by 4 grades of back extraction, obtained in the outlet of the 1st grade of stripping section containing Sm, Eu, Gd, Tb,
Dy, Ho, Er, Tm, Yb, Lu feed liquid (being represented with feed liquid b), yield 99%；
In after-fractionating extraction process, mixed extractant made from embodiment 2 is added to the 1st grade of extraction section, by before
State collection feed liquid a and be added to last 1 grade of extraction section, using 0.5mol/L hydrochloric acid solutions as cleaning solution, be added to washing section last 1
Level；Mixed extractant, feed liquid a, the flow-rate ratio of cleaning solution are 5：1：1.By 21 grades of extractions, 19 grades of washings, in the 1st grade of extraction section
Outlet obtains the feed liquid (being represented with feed liquid c) containing La, Ce, Pr, Nd, yield 99%；With the liquid of the last 1 grade of outflow of washing section
For organic phase, the 1st grade of stripping section is sent into, using 2mol/L hydrochloric acid solution as back extraction acid solution, is sent into last 1 grade of stripping section, it is organic
Mutually the flow-rate ratio with being stripped acid solution is 3:2, by 3 grades of back extraction, the chlorine that Y purity is 99.9% is obtained in the 1st grade of outlet of stripping section
Change yttrium feed liquid, yield 99%；Blank organic phase is collected from the last 1 grade of outlet of stripping section, its pH is 6.2, returns to extraction section the
One-level is reused；
The yttrium chloride feed liquid that above-mentioned collection obtains can be directly used for producing yittrium oxide product, collect obtained feed liquid b and
Feed liquid c can carry out the extraction of further rare earth element as needed.
Embodiment 11：Using the method for mixed extractant extract and separate yttrium from rare earth feed liquid
La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y concentration are 34.2g/L in rare earth feed liquid,
3.5g/L,8.7g/L,49.4g/L,7.3g/L,0.6g/L,7.2g/L,0.8g/L,6.4g/L,0.7g/L,3.7g/L,1.1g/
L,3.4g/L,0.9g/L,38.1g/L。
In the first fractional extraction process, mixed extractant made from embodiment 3 is added to the 1st grade of extraction section, will be dilute
Earth material liquid is added to last 1 grade of extraction section, using 0.9mol/L hydrochloric acid solutions as cleaning solution, is added to last 1 grade of washing section；It is mixed
It is 3 to close extractant, rare earth feed liquid, the flow-rate ratio of cleaning solution：1：1.By 11 grades of extractions, 9 grades of washings, in extraction section, the 1st grade goes out
Mouth obtains the feed liquid (being represented with feed liquid a) containing La, Ce, Pr, Nd, Y, yield 99%；With the liquid of the last 1 grade of outflow of washing section
For organic phase, the 1st grade of stripping section is sent into, using 1.5mol/L hydrochloric acid solution as back extraction acid solution, last 1 grade of stripping section is sent into, has
The flow-rate ratio of machine phase and back extraction acid solution is 3:1, by 3 grades of back extraction, obtained in the outlet of the 1st grade of stripping section containing Sm, Eu, Gd, Tb,
Dy, Ho, Er, Tm, Yb, Lu feed liquid (being represented with feed liquid b), yield 99%；
In after-fractionating extraction process, mixed extractant made from embodiment 3 is added to the 1st grade of extraction section, by before
State collection feed liquid a and be added to last 1 grade of extraction section, using 0.2mol/L hydrochloric acid solutions as cleaning solution, be added to washing section last 1
Level；Mixed extractant, feed liquid a, the flow-rate ratio of cleaning solution are 5：1：2.By 15 grades of extractions, 17 grades of washings, in the 1st grade of extraction section
Outlet obtains the feed liquid (being represented with feed liquid c) containing La, Ce, Pr, Nd, yield 99%；With the liquid of the last 1 grade of outflow of washing section
For organic phase, the 1st grade of stripping section is sent into, using 1.5mol/L hydrochloric acid solution as back extraction acid solution, last 1 grade of stripping section is sent into, has
The flow-rate ratio of machine phase and back extraction acid solution is 5:2, by 3 grades of back extraction, it is 99.9% to obtain Y purity in the 1st grade of outlet of stripping section
Yttrium chloride feed liquid, yield 99%；Blank organic phase is collected from the last 1 grade of outlet of stripping section, its pH is 5.9, returns to extraction section
The first order is reused；
The yttrium chloride feed liquid that above-mentioned collection obtains is directly used in production yittrium oxide product.
Embodiment 12：Using the method for mixed extractant extract and separate yttrium from rare earth feed liquid
La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y concentration are 18.2g/L in rare earth feed liquid,
0.5g/L,0.6g/L,18.4g/L,2.3g/L,0.6g/L,2.7g/L,0.8g/L,2.4g/L,0.3g/L,1.4g/L,0.5g/
L,1.1g/L,0.4g/L,20.7g/L。
In the first fractional extraction process, mixed extractant made from embodiment 4 is added to the 1st grade of extraction section, will be dilute
Earth material liquid is added to last 1 grade of extraction section, using 0.1mol/L hydrochloric acid solutions as cleaning solution, is added to last 1 grade of washing section；It is mixed
It is 2 to close extractant, rare earth feed liquid, the flow-rate ratio of cleaning solution：1：1.By 18 grades of extractions, 17 grades of washings, in extraction section, the 1st grade goes out
Mouth obtains the feed liquid (being represented with feed liquid a) containing La, Ce, Pr, Nd, Y, yield 99%；With the liquid of the last 1 grade of outflow of washing section
For organic phase, the 1st grade of stripping section is sent into, using 1mol/L hydrochloric acid solution as back extraction acid solution, is sent into last 1 grade of stripping section, it is organic
Mutually the flow-rate ratio with being stripped acid solution is 2:1, by 5 grades of back extraction, obtained in the outlet of the 1st grade of stripping section containing Sm, Eu, Gd, Tb, Dy,
Ho, Er, Tm, Yb, Lu feed liquid (being represented with feed liquid b), yield 99%；
In after-fractionating extraction process, mixed extractant made from embodiment 5 is added to the 1st grade of extraction section, by before
State collection feed liquid a and be added to last 1 grade of extraction section, using 0.4mol/L hydrochloric acid solutions as cleaning solution, be added to washing section last 1
Level；Mixed extractant, feed liquid a, the flow-rate ratio of cleaning solution are 4：1：0.7.By 17 grades of extractions, 15 grades of washings, in extraction section the 1st
Level outlet obtains the feed liquid (being represented with feed liquid c) containing La, Ce, Pr, Nd, yield 99%；With the liquid of the last 1 grade of outflow of washing section
Body is organic phase, is sent into the 1st grade of stripping section, using 1mol/L hydrochloric acid solution as back extraction acid solution, is sent into last 1 grade of stripping section, has
The flow-rate ratio of machine phase and back extraction acid solution is 3:2, by 3 grades of back extraction, it is 99.99% to obtain Y purity in the 1st grade of outlet of stripping section
Yttrium chloride feed liquid, yield 99%；Blank organic phase is collected from the last 1 grade of outlet of stripping section, its pH is 6.5, returns to extraction section
The first order is reused；
The yttrium chloride feed liquid that above-mentioned collection obtains is directly used in production yittrium oxide product.
Embodiment 13：Using the method for mixed extractant separation extract and separate yttrium from rare earth feed liquid
La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y concentration are 2.1g/L in rare earth feed liquid,
1.5g/L,1.7g/L,2.4g/L,1.3g/L,0.1g/L,4.1g/L,0.8g/L,5.4g/L,0.9g/L,2.7g/L,0.3g/L,
2.4g/L,0.2g/L,57.1g/L。
In the first fractional extraction process, mixed extractant made from embodiment 6 is added to the 1st grade of extraction section, will be dilute
Earth material liquid is added to last 1 grade of extraction section, using 0.7mol/L hydrochloric acid solutions as cleaning solution, is added to last 1 grade of washing section；It is mixed
It is 2 to close extractant, rare earth feed liquid, the flow-rate ratio of cleaning solution：1：0.5.By 10 grades of extractions, 11 grades of washings, in the 1st grade of extraction section
Outlet obtains the feed liquid (being represented with feed liquid a) containing La, Ce, Pr, Nd, Y, yield 99%；With the liquid of the last 1 grade of outflow of washing section
Body is organic phase, is sent into the 1st grade of stripping section, using 0.5mol/L hydrochloric acid solution as back extraction acid solution, is sent into last 1 grade of stripping section,
The flow-rate ratio of organic phase and back extraction acid solution is 1:1, by 4 grades of back extraction, obtained in the outlet of the 1st grade of stripping section containing Sm, Eu, Gd, Tb,
Dy, Ho, Er, Tm, Yb, Lu feed liquid (being represented with feed liquid b), yield 99%；
In after-fractionating extraction process, mixed extractant made from embodiment 7 is added to the 1st grade of extraction section, by before
State collection feed liquid a and be added to last 1 grade of extraction section, using 0.5mol/L hydrochloric acid solutions as cleaning solution, be added to washing section last 1
Level；Mixed extractant, feed liquid a, the flow-rate ratio of cleaning solution are 4：1：2.By 14 grades of extractions, 16 grades of washings, in the 1st grade of extraction section
Outlet obtains the feed liquid (being represented with feed liquid c) containing La, Ce, Pr, Nd, yield 99%；With the liquid of the last 1 grade of outflow of washing section
For organic phase, the 1st grade of stripping section is sent into, using 2.5mol/L hydrochloric acid solution as back extraction acid solution, last 1 grade of stripping section is sent into, has
The flow-rate ratio of machine phase and back extraction acid solution is 3:2, by 3 grades of back extraction, it is 99.99% to obtain Y purity in the 1st grade of outlet of stripping section
Yttrium chloride feed liquid, yield 99%；Blank organic phase is collected from the last 1 grade of outlet of stripping section, its pH is 5.7, returns to extraction section
The first order is reused；
The yttrium chloride feed liquid that above-mentioned collection obtains is directly used in production yittrium oxide product.
Claims (6)
- A kind of 1. mixed extractant for separating yttrium, it is characterised in that：By volume percentage, the composition of the mixed extractant For：Aphthenic acids 10~60%, basic extractant 10~50%, alcohols material 5~40%, diluent 10~60%.
- 2. the mixed extractant according to claim 1 for separating yttrium, it is characterised in that：The composition of the mixed extractant For：Aphthenic acids 20~40%, basic extractant 15~40%, alcohols material 10~30%, diluent 20~40%.
- 3. the mixed extractant according to claim 1 or 2 for separating yttrium, it is characterised in that：Described aphthenic acids is Acid number is 50~250mgKOH/g aphthenic acids.
- 4. the mixed extractant according to claim 1 or 2 for separating yttrium, it is characterised in that：Described alkaline extraction Agent is trialkyl tertiary amine or secondary carbon primary amine.
- 5. the mixed extractant according to claim 1 or 2 for separating yttrium, it is characterised in that：Described alcohols material For combination more than one or both of alcohol containing 2~8 carbon atoms.
- 6. the mixed extractant according to claim 1 or 2 for separating yttrium, it is characterised in that：Described diluent is Combination more than one or both of kerosene, hexamethylene, n-hexane and normal heptane.
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| CN110694300A (en) * | 2019-10-23 | 2020-01-17 | 金川集团股份有限公司 | Platinum-palladium efficient extraction and separation system and extraction and separation method thereof |
| CN113088692A (en) * | 2021-04-06 | 2021-07-09 | 鞍山昊旻稀土科技有限公司 | Extractant for extracting naphthenic acid and yttrium extraction process |
| CN113730954A (en) * | 2021-09-09 | 2021-12-03 | 福建省长汀金龙稀土有限公司 | Method for recovering isooctanol and sulfonated kerosene from waste organic of naphthenic acid system for extracting and separating yttrium |
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| CN106367622B (en) * | 2016-09-13 | 2018-12-07 | 南昌大学 | It is a kind of using aluminum sulfate as the ion adsorption type re efficient green extracting method of leaching agent |
| CN108486372B (en) * | 2018-02-13 | 2019-11-08 | 广西师范大学 | The removal methods of impurity in a kind of Rare Earth Mine leachate |
| CN109554556B (en) * | 2018-12-18 | 2021-02-26 | 广西师范大学 | Extraction separation method of rare earth elements |
| CN113384911B (en) * | 2021-08-06 | 2022-07-22 | 鞍山昊旻稀土科技有限公司 | Ester-decomposing distillation process of aged naphthenic acid extractant |
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| CN113730954A (en) * | 2021-09-09 | 2021-12-03 | 福建省长汀金龙稀土有限公司 | Method for recovering isooctanol and sulfonated kerosene from waste organic of naphthenic acid system for extracting and separating yttrium |
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