CN104946888B - The extract and separate extractant and its extraction separating method of a kind of yttrium - Google Patents
The extract and separate extractant and its extraction separating method of a kind of yttrium Download PDFInfo
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- CN104946888B CN104946888B CN201510270369.9A CN201510270369A CN104946888B CN 104946888 B CN104946888 B CN 104946888B CN 201510270369 A CN201510270369 A CN 201510270369A CN 104946888 B CN104946888 B CN 104946888B
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Abstract
The present invention relates to the extract and separate extractant and its extraction separating method of a kind of yttrium, the cation Wei quaternary phosphines base or quaternary ammonium group of the extractant, anion is secondary octyl phenoxy group substituted acetic acid salt.Extractant composition is simple, the organic phase stable performance of preparation, recycles, concentration, which has no, to be decreased obviously.Extractant is mixed to composition organic phase with diluent, the earth solution containing yttrium is efficiently extracted.Due to the distinctive the role of phase transfer of ionic liquid, back washing agent is easier to enter organic phase, substantially increases back extraction ratio.
Description
Technical field
The present invention relates to rare earth extraction separation field, more particularly, to a kind of extract and separate extractant of yttrium and its extraction
Separation method.
Background technology
Yittrium oxide is one of host materials of material such as fluorescence, microwave, laser, high technology ceramics, is widely used.But due to yttrium
Ionic radiusFall the erbium in lanthanide series sequenceNear, the chemical property of yttrium also with lanthanide series,
The chemical property of especially heavy lanthanide is very much like, it is difficult to is separated from each other.
In the prior art, separating yttrium is mainly using the extract and separate side with aphthenic acids (code name NA) for main body extractant
Method.It is as follows that long-term industrial applicability exposes aphthenic acids Process shortcoming：1. aphthenic acids is the byproduct of petroleum industry, into split pole
It is unstable；2. the pKa value of aphthenic acids is higher, be 7.57, worked under higher pH, easily with iron (III), thorium (IV), titanium
(IV), the impurity element of the high price such as zirconium (IV) forms solid naphthenate, so as to cause serious extractant to emulsify and lose；③
Aphthenic acids causes saponification number constantly to decline with phase modifying agent isooctanol slow reaction, needs the fresh extractant of regular replenishment even more
Change, produce largely discarded organic phase [Li Deqian, the Chemical Problems in Hydrometallurgical Industry of Rare Earths, chemical progress 7 (3), 209-
213,(1995)].Chinese invention patent 99118261.8 discloses a kind of liquid-liquid extraction method separating high-purity yttrium technique, and use is secondary
Octylphenoxy substituted acetic acid (code name CA12) and an alkali phosphorus (phosphine) acid or its single thio derivative (such as P204, P507,
Cyanex 272, Cyanex302 etc.) mixture as extractant separate yttrium, solve cycloalkanes acid system emulsification problem,
But also there is the problem of organic phase concentration decline in the above method.
The content of the invention
It is an object of the invention to overcome above-mentioned deficiency of the prior art, there is provided a kind of extract and separate extraction of yttrium
Agent, the separation height of the extractant, extraction phenomenon are good, and organic phase is stable, is recycled for a long time, under concentration has no obvious
Drop.
It is another object of the present invention to provide a kind of extraction separating method of efficient yttrium.
In view of this, the present invention provides following technical scheme：
The extract and separate extractant of a kind of yttrium, it is characterised in that the extractant is the ionic liquid shown in following formula (1)
One or more mixtures in based compound：
Formula (1)
Wherein,
X is P or N；
R1、R2、R3And R4It is identical or different, it is independently from each other substituted or unsubstituted branched-chain or straight-chain alkyl, substitution
Or unsubstituted aryl；The substituent is branched-chain or straight-chain alkyl, side chain or unbranched alkoxy or halogen.
According to the present invention, R1、R2、R3And R4In the branched-chain or straight-chain alkyl be preferably C1-C20Side chain or straight chain
Alkyl, also preferably C1-15Branched-chain or straight-chain alkyl, more preferably methyl, ethyl, normal-butyl, n-hexyl, positive decyl, the tetradecane
Base；The aryl is preferably C6-20Aryl, more preferably phenyl or naphthyl, more preferably phenyl.
According to the present invention, R1、R2、R3And R4In two or three or four groups it is identical.Such as R1、R2、R3And R4In
Three are n-hexyl, and another is n-tetradecane base；Or R1、R2、R3And R4All it is normal-butyl.
The present invention also provides following technical scheme：
A kind of extraction separating method of yttrium, comprises the following steps：
(1) above-mentioned extractant is mixed to composition organic phase with diluent；
(2) organic phase obtained by step (1) is mixed with the solution of the rare earth containing yttrium, carries out selective extraction, stay yttrium
In aqueous phase, rare earth enters organic phase.
Preferably, methods described is further comprising the steps of：
(3) organic phase obtained by step (2) is stripped using inorganic acid, the rare earth in organic phase is entered water
Phase.
Preferably, the organic phase after being stripped in the step (3) can be recycled and reused for replacing the step in step (2)
(1) organic phase obtained by.Preferably, the number of the reuse is at least 15 times.
Preferably, the volume ratio of the extractant in the step (1) and diluent is 1~50：99~50, also preferably 10
~40：90~60, or preferably 20~30：80~70.
Preferably, one or more of the diluent in alkane or aromatic hydrocarbons.Preferably, the alkane is selected from heptan
One or more in alkane, octane, hexadecane, aviation kerosine and 260# solvent kerosene, the aromatic hydrocarbons are selected from benzene, toluene and diformazan
One or more in benzene.
Preferably, the one kind of the inorganic acid in hydrochloric acid, nitric acid or sulfuric acid.More preferably hydrochloric acid or nitric acid, it is optimal
Elect hydrochloric acid as.
According to the present invention, the molar concentration of the inorganic acid is preferably between 0.01- between 0.005-1.0 mol/Ls
Between 0.5 mol/L.
Compared with prior art, the invention provides the extract and separate extractant and its extraction separating method of a kind of yttrium,
Its advantage is：1. this extractant composition is simple, the organic phase stable performance of preparation, the turnover rate of extractant is less than 0.5%.2. this
Good separating effect of the extractant to yttrium.3. due to the distinctive the role of phase transfer of ionic liquid, back washing agent is easier to enter organic phase, greatly
Back extraction ratio is improved greatly, the concentration of the back washing agent used is far below 2.0 mol/L of the prior art, and optimal concentration is 0.2
Mol/L can realizes the back extraction ratio close to 100%.4. the present invention also uses ionic liquid saponification, do not produced in extraction process
Ammonia nitrogen waste water.Therefore, the invention provides a kind of composition simply and stable performance extractant, and it is a kind of efficiently yttrium extraction
Take separation method.
Brief description of the drawings
Fig. 1 is for extractant [P6,6,6,14] [CA12] of the invention from the extractant CA12 of prior art to different rare earths
Separation.
Embodiment
As it was previously stated, the invention provides the extract and separate extractant and its extraction separating method of a kind of yttrium, extraction side
Method comprises the following steps：(1) above-mentioned extractant is mixed to composition organic phase with diluent；(2) will be organic obtained by step (1)
Mutually mixed with the solution of the rare earth containing yttrium, carry out selective extraction, yttrium is stayed in aqueous phase, other rare earths enter organic phase.It is preferred that
, methods described further comprises that (3) are stripped using inorganic acid to the organic phase obtained by step (2), makes in organic phase
Rare earth enter aqueous phase.
In the present invention, the cation of ionic liquid based compound is selected from quaternary phosphine base or quaternary ammonium group, and anion is secondary octyl
Phenoxy group substituted acetic acid root, the source of the presoma of the cation and anion is without limiting, for example, the anion comes
From secondary octyl phenoxy group substituted acetic acid salt.Preferably according to the extract and separate extractant of the described yttrium of acid-base neutralization method synthesis
(i.e. described ionic liquid based compound).
In the present invention, the extractant and diluent are mixed to get the hybrid mode of organic phase without restriction, ability
Hybrid mode known to field technique personnel.
The solution of the rare earth containing yttrium used in the present invention, can be the salpeter solution of the rare earth containing yttrium, or containing yttrium
Rare earth hydrochloric acid solution, the present invention to this without limit.
The temperature of extraction of the present invention is preferably 20 DEG C~35 DEG C, more preferably 23 DEG C~30 DEG C；The extraction time
Preferably 5~10min.The back extraction temperature is preferably 20 DEG C~35 DEG C, more preferably 23 DEG C~30 DEG C；During the back extraction
Between be preferably 5~10min.
After the completion of extraction separation process, the mixed rare-earth elements in raffinate or stripping workshop that the present invention obtains are preferably sharp
It is measured with ICP-MS methods, referring in particular to the 8th part of GB/T 18114.8-2010 rare earth ore concentrates chemical analysis methods 15
Rare earth oxide matches somebody with somebody the measure of component.
Rare Earth Elements Determination uses arsenazo (III) colorimetric method for determining.
The calculation formula of extraction yield (E), distribution ratio (D), back extraction ratio (S) and the separation (β) used is as follows：
Wherein, [M]t[M]aThe balance of aqueous phase rare earth ion respectively after the initial concentration of aqueous phase rare earth ion and extraction
Concentration, [M]aq,a[M]org,tRespectively strip liquor middle rare earth concentration and organic phase rare earth concentration.D1And D2It is extractant to difference
Two kinds of rare earths distribution ratio.
The present invention is described in further detail with accompanying drawing with reference to embodiments.But skilled in the art realises that
Protection scope of the present invention is not limited only to following examples.According to present disclosure, those skilled in the art will recognize that
To in the case where not departing from technical characteristic and the scope given by technical solution of the present invention, embodiment described above is made perhaps
Change and modifications belongs to protection scope of the present invention more.Material therefor in following embodiments, it is business unless otherwise specified
On the product that is commercially available.
Embodiment 1
The synthesis of [N4,4,4,4] [CA12]
In 125ml separatory funnels, 0.006 mole 4-butyl amine (being designated as [N4,4,4,4] Br) is added to 40ml
In methanol, 75ml strong-base anion-exchange resins are added, tetrabutylphosphoniuhydroxide hydroxide amine (being designated as [N4444] OH) solution is made.
0.006 mole of secondary octyl phenoxy group substituted acetic acid (code name CA12) is added in this solution, and gained mixture stirs at room temperature
6h is mixed, until solution is changed into neutral, is screwed out at 70 DEG C first alcohol and water with Rotary Evaporators, product is 70 in vacuum drying chamber
DEG C dry 12h, obtain thick liquid [N4,4,4,4] [CA12].Yield reaches 95%.
Embodiment 2
The synthesis of [P6,6,6,14] [CA12]
In 250ml separatory funnels, by 0.012 mole of Ji Ji Phosphonium of tetradecyl chloride base three (be designated as [P6,6,6,14] Br,
Code name CYPHOS IL 101) it is added in 80ml methanol, 150ml strong-base anion-exchange resins are added, hydroxide is made
The Ji Ji Phosphonium of myristyl three (being designated as [P6,6,6,14] OH) solution.0.012 mole of secondary octyl phenoxy group is added in this solution
6h is stirred at room temperature in substituted acetic acid (code name CA12), gained mixture, until solution is changed into neutral, with Rotary Evaporators by first
Alcohol and water screws out at 70 DEG C, product 70 DEG C of dry 12h in vacuum drying chamber, obtains thick liquid [P6,6,6,14]
[CA12].Yield reaches 94%.
Embodiment 3
Prepare organic phase：[P6,6,6,14] [CA12] that is synthesized in embodiment 2 is mixed with toluene, forms organic phase,
The concentration of [P6,6,6,14] [CA12] is 0.10 mol/L.
Preparation raw material liquid：The solution of yttrium, holmium, erbium, thulium, ytterbium and lutetium is taken respectively, adds watery hydrochloric acid, it is dense to be configured to single rare earth
Spending the material liquid containing yttrium for 0.06 mol/L, wherein NaCl is 0.5 mol/L, pH 3.2, total concentration is 0.36 mole/
Rise.
By organic phase and material liquid by volume 1:1 mixing, is extracted at room temperature, and extraction series is 1 grade.Extraction finishes
Afterwards, extraction yield E, distribution ratio D and separation β are calculated.Extraction yield E and distribution ratio D is shown in Table 1, and separation β is shown in Fig. 1.By 15
Secondary recycling, organic phase stable performance, extraction phenomenon are good.
Table 1
Comparative example 1
Prepare organic phase：The secondary octyl phenoxy group substituted acetic acid CA12 of commercialization is mixed with isooctanol, toluene, composition has
Machine phase, CA12 concentration is 0.10 mol/L, and the volumetric concentration of isooctanol is 2%.
Preparation raw material liquid：With embodiment 3.
By organic phase and material liquid by volume 1:1 mixing, is extracted at room temperature, and extraction series is 1 grade.Extraction finishes
Afterwards, extraction yield E, distribution ratio D and separation β are calculated.Extraction yield E and distribution ratio D is shown in Table 2, and separation β is shown in Fig. 1.By 15
Secondary recycling, organic phase concentration have dropped 25%.
Table 2
| CA12 systems | Y | Ho | Er | Tm | Yb | Lu |
| E% | 5.3 | 6.1 | 7.3 | 9.1 | 9.5 | 2.0 |
| D | 0.056 | 0.065 | 0.079 | 0.100 | 0.105 | 0.021 |
As shown in figure 1, [P6,6,6,14] [CA12] system is excellent to the selectivity of yttrium.Under this experiment condition, organic phase
The stability of selectivity and organic phase to yttrium is substantially better than CA12 systems.
Embodiment 4
Prepare organic phase：By synthesized in [N4,4,4,4] [CA12] that is synthesized in embodiment 1 and embodiment 2 [P6,6,6,
14] [CA12] is with mol ratio 1：1 carries out mixing composition mixed extractant.Mixed extractant is mixed with toluene, forms organic phase,
The concentration of [N4,4,4,4] [CA12] is 0.05 mol/L, and the concentration of [P6,6,6,14] [CA12] is 0.05 mol/L.
Other steps are the same as embodiment 3.
Extraction yield E, distribution ratio D and separation the β difference of above-mentioned extraction are similar to Example 3.
Embodiment 5~7
Prepare organic phase：[P6,6,6,14] [CA12] that is synthesized in embodiment 2 is mixed with toluene, forms organic phase,
The concentration of [P6,6,6,14] [CA12] is 0.07 mol/L.
Preparation raw material liquid：The solution of yttrium is taken, adds watery hydrochloric acid, is configured to the original containing yttrium that yttrium concentration is 0.002 mol/L
Feed liquid, wherein NaCl are 0.5 mol/L, pH 3.2.
By above-mentioned [P6,6,6,14] [CA12] organic phase and the material liquid containing yttrium by volume 1:1 mixing, is extracted
Take, the concentration for making to load yttrium in organic phase is 0.0012 mol/L.By the anti-stripping agent of load organic phases and various concentrations with body
Product is than being 1:1 mixing, is stripped at room temperature.The anti-stripping agent is hydrochloric acid, and its concentration is respectively 0.01,0.02,0.2 to rub
You/liter.After back extraction, stripping rate S is calculated.As a result show, the back extraction of 0.01,0.02 and 0.2 mol/L anti-stripping agent
Rate is taken to respectively reach 92%, 94% and 99%.
Embodiment 8~10
[N4,4,4,4] [CA12] extractant being changed in embodiment 1, other are identical with embodiment 5~7, as a result table
Bright, the stripping rate of 0.01,0.02 and 0.2 mol/L anti-stripping agent respectively reaches 90%, 93% and 98%.
Embodiment 11~13
Prepare organic phase：[P6,6,6,14] [CA12] that is synthesized in embodiment 2 is mixed with toluene, forms organic phase,
The concentration of [P6,6,6,14] [CA12] is 0.03 mol/L.
Preparation raw material liquid：The solution of yttrium is taken, adds watery hydrochloric acid, is configured to yttrium concentration respectively as 0.002 mol/L, 0.004
The material liquid of mol/L and 0.006 mol/L, wherein NaCl are 0.5 mol/L, pH 3.2.
By above-mentioned [P6,6,6,14] [CA12] organic phase respectively with 0.002 above-mentioned mol/L, 0.004 mol/L
The material liquid containing yttrium with 0.006 mol/L is with volume ratio 1：1 mixing, is extracted, determines the turnover rate of extractant.As a result
Show, in the solution after extraction, the concentration of total phosphorus is respectively 0.72 mg/litre, 0.73 mg/litre and 0.77 mg/litre, is less than
The discharge standard (the indirect mg/litre of emission limit 5 of phosphorus) of phosphorus in rare-earth industry pollutant as defined in GB/T 26451-2011.
Embodiment 14~16
[N4,4,4,4] [CA12] extractant being changed in embodiment 1, other are identical with embodiment 11~13, as a result table
Bright, in the solution after extraction, the concentration of total nitrogen is respectively 0.75 mg/litre, 0.75 mg/litre and 0.80 mg/litre, is less than
The discharge standard (the indirect mg/litre of emission limit 70 of total nitrogen) of nitrogen in rare-earth industry pollutant as defined in GB26451-2011.
Claims (16)
1. the extract and separate extractant of a kind of yttrium, it is characterised in that the extractant is the ion liquid-based shown in following formula (1)
One or more mixtures in compound：
Wherein,
X is P or N；
R1、R2、R3And R4It is identical or different, it is independently from each other normal-butyl, n-hexyl, myristyl.
2. extractant according to claim 1, it is characterised in that R1、R2、R3And R4In two or three or four groups
It is identical.
3. extractant according to claim 2, it is characterised in that R1、R2、R3And R4In three be n-hexyl, another
For n-tetradecane base；Or R1、R2、R3And R4All it is normal-butyl.
4. a kind of extraction separating method of yttrium, comprises the following steps：
(1) extractant described in claim any one of 1-3 is mixed to composition organic phase with diluent；
(2) organic phase obtained by step (1) is mixed with the solution of the rare earth containing yttrium, carries out selective extraction, yttrium is stayed in water
Phase, rare earth enter organic phase.
5. extraction separating method according to claim 4, it is characterised in that methods described is further comprising the steps of：
(3) organic phase obtained by step (2) is stripped using inorganic acid, the rare earth in organic phase is entered aqueous phase.
6. extraction separating method according to claim 5, it is characterised in that organic after being stripped in the step (3)
Mutually it is recycled and reused for replacing the organic phase obtained by the step (1) in step (2).
7. extraction separating method according to claim 6, it is characterised in that the number of the reuse is at least 15
It is secondary.
8. according to the extraction separating method described in claim any one of 4-7, it is characterised in that the extraction in the step (1)
The volume ratio of agent and diluent is 1~50：99~50.
9. extraction separating method according to claim 8, it is characterised in that extractant and dilution in the step (1)
The volume ratio of agent is 10~40：90~60.
10. according to the extraction separating method described in claim any one of 4-7, it is characterised in that the diluent is selected from alkane
Or the one or more in aromatic hydrocarbons.
11. extraction separating method according to claim 10, it is characterised in that the alkane is selected from heptane, octane, 16
One or more in alkane, aviation kerosine and 260# solvent kerosene, one kind in benzene, toluene and dimethylbenzene of the aromatic hydrocarbons or
It is a variety of.
12. according to the extraction separating method described in claim any one of 5-7, it is characterised in that the inorganic acid be selected from hydrochloric acid,
One kind in nitric acid or sulfuric acid.
13. extraction separating method according to claim 12, it is characterised in that the inorganic acid is hydrochloric acid or nitric acid.
14. extraction separating method according to claim 13, it is characterised in that the inorganic acid is hydrochloric acid.
15. according to the extraction separating method described in claim any one of 5-7, it is characterised in that the inorganic acid it is mole dense
Degree is between 0.005-1.0 mol/Ls.
16. extraction separating method according to claim 15, it is characterised in that the molar concentration of the inorganic acid between
Between 0.01-0.5 mol/Ls.
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| CN201510270369.9A CN104946888B (en) | 2015-05-25 | 2015-05-25 | The extract and separate extractant and its extraction separating method of a kind of yttrium |
| CA2925149A CA2925149C (en) | 2015-05-25 | 2016-03-24 | Extractant and method for extracting and separating yttrium |
| US15/081,344 US10428405B2 (en) | 2015-05-25 | 2016-03-25 | Extractant and method for extracting and separating yttrium |
| AU2016202668A AU2016202668B2 (en) | 2015-05-25 | 2016-04-27 | Extractant and method for extracting and separating yttrium |
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| CA2925149C (en) | 2015-05-25 | 2022-10-04 | Xiamen Institute Of Rare Earth Materials | Extractant and method for extracting and separating yttrium |
| CN105238926B (en) * | 2015-11-13 | 2017-07-21 | 厦门稀土材料研究所 | A kind of extraction separating method of yttrium |
| CN108456792B (en) * | 2017-02-17 | 2019-11-26 | 厦门稀土材料研究所 | A kind of rare earth extraction separation extractant and preparation method thereof and extraction separating method |
| CN109811149A (en) * | 2017-11-20 | 2019-05-28 | 厦门稀土材料研究所 | A kind of back extraction and regeneration method of extracting and separating rear earth ionic liquid |
| CN108383713B (en) * | 2018-03-09 | 2020-08-21 | 厦门熙途科技有限公司 | Organic precipitator and preparation method and application thereof |
| CN112458282B (en) * | 2019-09-06 | 2023-03-28 | 中国科学院长春应用化学研究所 | Use and method of phosphoryl carboxylic acids or salts thereof for separating yttrium |
| CN114540619B (en) * | 2020-11-25 | 2024-02-13 | 厦门稀土材料研究所 | Functional ionic liquid and preparation method and application thereof |
| CN112662872B (en) * | 2020-12-03 | 2022-10-11 | 江西理工大学 | Extraction method of oxalic acid-containing solution |
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