CN109179479A - The method for extracting scandium fluoride - Google Patents
The method for extracting scandium fluoride Download PDFInfo
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- CN109179479A CN109179479A CN201811143112.7A CN201811143112A CN109179479A CN 109179479 A CN109179479 A CN 109179479A CN 201811143112 A CN201811143112 A CN 201811143112A CN 109179479 A CN109179479 A CN 109179479A
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- scandium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/265—Fluorides
Abstract
The invention discloses a kind of methods for extracting scandium fluoride.Method includes the following steps: S1, carries out scandium extraction to inorganic acid solution containing scandium using the organic solvent solution of the extractant containing acidic organo phosphorus, obtains the organic phase containing scandium；S2 carries out carrying out washing treatment to the organic phase containing scandium to remove impurity；S3 is added HF and/or NaF solution into the organic phase containing scandium after removing impurity and is stripped, and scandium complex anion solution and unloaded organic phase are obtained after Liquid liquid Separation, the pH value of hydrochloric acid conditioning solution is added, into scandium complex anion solution to generate ScF3It precipitates, obtains ScF after separation of solid and liquid3Precipitating and mother liquor of precipitation of ammonium；S4, by ScF3Scandium fluoride product is obtained after washing of precipitate, drying.It applies the technical scheme of the present invention, shortens operating process, reduce back extraction acid, neutralize the consumption of raw materialss such as alkali, water, oxalic acid, reduce operating cost, be conducive to be applied to industrial production.
Description
Technical field
The present invention relates to metallurgical technology fields, in particular to a kind of method for extracting scandium fluoride.
Background technique
Scandium fluoride can do optical material and molten-salt electrolysis, metallothermic processes prepare the weight of scandium metal and its alloy
Want raw material.Acidic organo phosphorus extractant has good effect of extracting to scandium (Sc), and extraction efficiency is high, and can be by scandium and impurity member
Plain separation well, but scandium (Sc) is difficult to be stripped from the organic solution of the extractant containing acidic organo phosphorus, generally requires very
High acidity (sulfuric acid solution of such as 600g/L or more) and repeatedly it is stripped extract operation.And the highly acidity scandium solution that back extraction obtains
Middle concentration impurity ion is higher, needs to be further purified operation, and common method is that oxalic acid solution is added at a lower level of acidity
Precipitating generates oxalic acid scandium precipitating, and then oxalic acid scandium precipitating is dry to generate scandium oxide, then by scandium oxide product acid dissolution, then
It is precipitated to obtain scandium fluoride (ScF with villiaumite such as NaF solution3) precipitating, therefore, it is necessary to expend a large amount of acid-base solution to carry out instead
The reactions such as extraction, precipitating, neutralization, and consume the high oxalic acid reagent of a large amount of prices, expend energy.
Summary of the invention
The present invention is intended to provide a kind of method for extracting scandium fluoride, to solve to extract scandium fluoride operating process in the prior art
Technical problem long, consumption of raw materials is big.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of method for extracting scandium fluoride.The party
Method carries out scandium to inorganic acid solution containing scandium using the organic solvent solution of the extractant containing acidic organo phosphorus the following steps are included: S1
Extraction obtains the organic phase containing scandium；S2 carries out carrying out washing treatment to the organic phase containing scandium to remove impurity；S3, to except impurity elimination
HF and/or NaF solution is added in the organic phase containing scandium after matter to be stripped, it is molten that scandium complex anion is obtained after Liquid liquid Separation
Liquid and unloaded organic phase, are added the pH value of hydrochloric acid conditioning solution, into scandium complex anion solution to generate ScF3Precipitating, solid-liquid
ScF is obtained after separation3Precipitating and mother liquor of precipitation of ammonium；S4, by ScF3Scandium fluoride product is obtained after washing of precipitate, drying.
Further, in S3, F in HF and/or NaF solution-In ion and inorganic acid solution containing scandium the amount of the substance of scandium it
Than being greater than 3 less than 4.5.
Further, acidic organo phosphorus extractant is selected from by di-(2-ethylhexyl)phosphoric acid, the mono- 2- of 2- ethylhexyl phosphoric acid
One of group of ethylhexyl and Cyanex272 extractant composition is a variety of.
Further, the organic extractant in the organic solvent solution of the extractant containing acidic organo phosphorus is that density is less than water
Alkanes or at least one of its mixture or arene；Preferably, alkanes or its mixture include normal heptane, just
Hexane and kerosene；Preferably, arene includes benzene and toluene.
Further, the concentration of the extractant containing acidic organo phosphorus is in the organic solvent solution of the extractant containing acidic organo phosphorus
0.01mol/L~4mol/L.
Further, inorganic acid solution containing scandium is sulfuric acid solution, hydrochloric acid solution or nitric acid solution containing scandium.
Further, the organic solvent solution of the extractant containing acidic organo phosphorus is with the volume ratio of the inorganic acid solution containing scandium
(1:20)~(1:1).
Further, in the organic solvent solution and S3 of the extractant containing acidic organo phosphorus HF and/or NaF solution volume ratio
For (1:20)~(20:1).
Further, S4 includes: respectively with ethyl alcohol and water washing ScF3Precipitating.
It further, is 20~40 DEG C with the temperature of ethanol washing, the temperature being washed with water is 50~90 DEG C.
Further, in S2, cleaning solution used in carrying out washing treatment is the aqueous hydrochloric acid solution or 0.1~1mol/ of 0.1~2mol/L
The aqueous sulfuric acid of L.
Further, the mother liquor of precipitation of ammonium in S3 is added after HF and/or NaF and returns to back extraction processing step use, it is unloaded
Organic phase returns to scandium extraction processing step in S1 and uses.
Further, scandium extraction and back extraction processing in mixing use mechanical mixture or ultrasonic wave mixing with accelerate to react into
Degree.
Further, the reaction temperature of back extraction is 20~70 DEG C, preferably 25~45 DEG C.
Further, in S1, in the organic solvent solution of the extractant containing acidic organo phosphorus acidic organo phosphorus extractant with contain
The ratio between amount of substance of scandium is greater than 3 less than 20 in scandium inorganic acid solution.
Further, scandium fluoride is precipitated in S4 dry to generate the temperature of scandium fluoride product as 90~105 DEG C.
It applies the technical scheme of the present invention, scandium is extracted from solution containing scandium, F is then added-To realize scandium quilt in organic phase
It is stripped simultaneously and precipitating, so that scandium is able to enrichment and separation, is made simultaneously so that scandium ion is directly translated into scandium fluoride precipitating
It is standby to have obtained scandium fluoride product, operating process is shortened, back extraction acid is reduced, neutralizes the consumption of raw materialss such as alkali, water, oxalic acid, reduce behaviour
Make expense, is conducive to be applied to industrial production.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the flow diagram of extraction scandium fluoride according to an embodiment of the present invention.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
For scandium oxide is extracted in the prior art, the invention proposes following technical proposals:
A kind of typical embodiment according to the present invention provides a kind of method for extracting scandium fluoride.Should the following steps are included:
S1 carries out scandium extraction to inorganic acid solution containing scandium using the organic solvent solution of the extractant containing acidic organo phosphorus, and acquisition contains scandium
Organic phase；S2 carries out carrying out washing treatment to the organic phase containing scandium to remove impurity；S3, to remove after impurity containing scandium
HF and/or NaF solution is added in organic phase to be stripped, scandium complex anion solution is obtained after Liquid liquid Separation and zero load is organic
The pH value of hydrochloric acid conditioning solution is added, into scandium complex anion solution to generate ScF in phase3It precipitates, is obtained after separation of solid and liquid
ScF3Precipitating and mother liquor of precipitation of ammonium；S4, by ScF3Scandium fluoride product is obtained after washing of precipitate, drying.
It extracts reaction as (HA represents extractant, footnote(o)Represent organic phase):
Sc3++3HA(o)→ScA3(o)+3H+
It precipitates back extraction reaction are as follows:
ScA3(o)+3NaF→3NaA(o)+ScF3↓, ScA3(o)+3HF→3HA(o)+ScF3↓
It applies the technical scheme of the present invention, (is extracted containing acidic organo phosphorus using the organic phase of the extractant containing acidic organo phosphorus
The organic solvent solution of agent) scandium extraction processing is carried out to feed liquid containing scandium (inorganic acid solution containing scandium), it is negative containing scandium to obtain
Carry organic phase；From impurity of the organic phase carrying out washing treatment to remove while extract containing scandium；By organic addition after above-mentioned removal of impurities
Enter HF and/or NaF solution to be stripped, to generate scandium fluoride (ScF3) precipitating；By scandium fluoride washing of precipitate, the drying of generation
To generate scandium fluoride product.Using this method can effectively scandium fluoride be extracted in enrichment from solution containing scandium.
Preferably, in S3, F in HF and/or NaF solution-The ratio between the amount of substance of scandium in ion and inorganic acid solution containing scandium
Greater than 3 less than 4.5, there is utilization to be adequately precipitated out scandium.
Preferably, acidic organo phosphorus extractant is selected from by di-(2-ethylhexyl)phosphoric acid, the mono- 2- second of 2- ethylhexyl phosphoric acid
One of group of base hexyl ester and Cyanex272 extractant composition is a variety of；The organic solvent of the extractant containing acidic organo phosphorus
Organic extractant in solution is that density is less than the alkanes of water or at least one of its mixture or arene；More preferably
, alkanes or its mixture include normal heptane, n-hexane and kerosene；It is furthermore preferred that arene includes benzene and toluene.
In order to advanced optimize the performance of extractant, the organic solvent solution of the extractant containing acidic organo phosphorus (is also known as extracted
Agent) in the extractant containing acidic organo phosphorus concentration be 0.01mol/L~4mol/L.
A kind of typical embodiment according to the present invention, inorganic acid solution containing scandium are sulfuric acid solution, hydrochloric acid solution containing scandium
Or nitric acid solution can contain other metal ions, such as Ca certainly in inorganic acid solution containing scandium2+、Mg2+、Mn2+、Ni2+、Al3 +、Fe3+、Cr3+。
Preferably, the volume ratio of the organic solvent solution of the extractant containing acidic organo phosphorus and the inorganic acid solution containing scandium be (1:
20)~(1:1) is conducive to scandium in this proportional region and sufficiently and is efficiently extracted.Preferably, extract containing acidic organo phosphorus
The volume ratio for taking HF and/or NaF solution in the organic solvent solution and S3 of agent is (1:20)~(20:1).
A kind of typical embodiment according to the present invention, S4 include: respectively with ethyl alcohol and water washing ScF3Precipitating, in order to
The organic matter and water-solubility impurity of adsorption are removed respectively.Preferably, ethanol washing temperature is 20~40 DEG C, water washing temperature
It is 50~90 DEG C.
Preferably, in S2, cleaning solution used is the aqueous hydrochloric acid solution of 0.1~2mol/L or the sulfuric acid water of 0.1~1mol/L
Solution.
A kind of typical embodiment according to the present invention returns to back extraction after HF and/or NaF is added in the mother liquor of precipitation of ammonium in S3
Processing step is taken to use, unloaded organic phase returns to scandium extraction processing step in S1 and uses, be conducive to the abundant recycling of raw material,
Reduce production cost.
Churned mechanically mixing is all made of in a kind of typical embodiment according to the present invention, scandium extraction and back extraction processing
Mode accelerates extent of reaction.
Preferably, the reaction temperature of back extraction is 20~70 DEG C, preferably 25~45 DEG C.
Preferably, in S1, in the organic solvent solution of the extractant containing acidic organo phosphorus acidic organo phosphorus extractant with contain scandium
The ratio between amount of substance of scandium is greater than 3 less than 20 in inorganic acid solution, is conducive to scandium in this proportional region by abundant and efficient
It extracts.
Preferably, scandium fluoride is precipitated in S4 dry to generate the temperature of scandium fluoride product as 90~105 DEG C.
A kind of typical embodiment according to the present invention, as shown in Figure 1, this method comprises: extracting using containing acidic organo phosphorus
The organic phase of agent is taken to carry out scandium extraction processing to feed liquid containing scandium, to obtain the load organic phases containing scandium, control extractant is dense
Degree etc. reaction conditions, and make organic phase volume be less than water phase volume so that scandium be enriched with and with foreign ion (such as Ca2+、
Mg2+、Mn2+、Ni2+、Al3+、Fe3+、Cr3+) separation；From the organic phase carrying out washing treatment containing scandium, it can remove while extracting
The a small amount of foreign ion for taking or carrying secretly, so that scandium is further purified；By organic after above-mentioned removal of impurities be added to HF, NaF solution into
Row precipitating back extraction, to generate scandium fluoride ScF3Precipitating, research find that strippant concentration can be precipitated by control, temperature, have
The reaction conditions such as machine phase/water phase volume ratio keep the scandium fluoride that stripping efficiency is high, organic phase effect separated from the water is good, generates heavy
Form sediment (ScF3) have high deposition efficiency and be conducive to the filtering of lower step；By scandium fluoride precipitating respectively with second alcohol and water in selected temperature
The lower washing of degree, to remove the organic matter and water-solubility impurity of adsorption respectively, scandium is further purified, and after washing
Scandium fluoride precipitating has preferably by strainability；The scandium fluoride washing of generation, precipitating is dry to generate scandium fluoride product.With
When HF, NaF solution are stripped, under optimal conditions (including concentration, temperature, organic phase: water phase volume ratio) it has been extracted into
Scandium and HF, NaF in machine phase generate scandium fluoride and precipitate (ScF3), scandium fluoride can form preferable crystal habit, and hydrophily is strong,
Scandium is easy to enter aqueous phase solution in the form of precipitating, so that stripping efficiency is high, organic phase effect separated from the water is good, can be with
Using mixed settler extractor carry out extraction and separation continuous operation, scandium fluoride precipitating can using traditional solid-liquid separating equipment into
Row separation, thus, it is conducive to be applied to industrial production.
Beneficial effects of the present invention are further illustrated below in conjunction with embodiment.
Embodiment 1
P507 extractant (the mono- 2- ethylhexyl of 2- ethylhexyl phosphoric acid), NaF back extraction
In mixed settler extractor, it is 1:1 according to organic solution, the ratio of liquor capacity containing scandium, is extracted with containing 1mol/LP507
The solution of the kerosin for taking agent, scandium chloride and 1mol/L hydrochloric acid from the scandium containing 0.3mol/L is mixed to extract in solution containing scandium
Scandium；
The organic phase for loading scandium is washed with 1mol/L aqueous hydrochloric acid solution, to remove the impurity element extracted jointly；
Volume ratio (organic solution, aqueous solution volume ratio) according to extractant organic solution, back extraction agent solution is 1:1, will
The organic phase of washing back loading scandium is mixed with the stripping agent aqueous solution (water phase) of the NaF containing 1mol/L, reaction temperature 50
DEG C, to carry out back extraction reaction, the scandium fluoride precipitating of generation exports outflow in water phase and from water phase；Unloaded scandium it is organic
It is mutually separated with solution, and returns to extraction step recycling；
By the hydrofluorination scandium precipitating of generation with water phase by isolated by vacuum filtration, the scandium fluoride being enriched with is precipitated；By fluorine
Change after NaF is added in scandium mother liquor of precipitation of ammonium and returns to scandium back extraction processing step use；Scandium fluoride precipitating is used into ethyl alcohol and water washing respectively,
Wash temperature is 30 DEG C and 80 DEG C, to remove the organic matter and water-solubility impurity of adsorption respectively.
By scandium fluoride ScF3100 DEG C of dryings are deposited in generate scandium fluoride product, wherein scandium extraction recovery can achieve
95%.
Embodiment 2
P204 extractant (di-(2-ethylhexyl)phosphoric acid), HF back extraction
It is 1:10 according to organic solution, the ratio of liquor capacity containing scandium, with containing in the reaction kettle that band is stirred effect
The n-heptane solution of 1mol/L (di-(2-ethylhexyl)phosphoric acid ester) extractant (P204 extractant) from scandium containing 0.02mol/L and
Extracting scandium in 0.5mol/L sulfuric acid solution；The organic phase for loading scandium is washed with 0.5mol/L aqueous sulfuric acid, according to extraction
Taking agent organic solution, the volume ratio (organic solution: aqueous solution volume ratio) of precipitating back extraction agent solution is 10:1, will be negative after washing
The organic phase for carrying scandium is mixed with the stripping agent aqueous solution (water phase) containing 7mol/LHF, carries out back extraction reaction, and generate fluorine
Change scandium precipitating；Scandium fluoride precipitating is used into ethyl alcohol and water washing respectively, wash temperature is 40 DEG C and 90 DEG C；Scandium fluoride ScF3 is precipitated
It is dry to generate scandium fluoride product at 105 DEG C.
The organic phase of unloaded scandium separates in mixed settler extractor with precipitating stripping agent aqueous solution, and the scandium fluoride of generation is heavy
It forms sediment to export in water phase and together with mother liquor of precipitation of ammonium from water phase and flow out；The scandium fluoride of generation is precipitated and is passed through with mother liquor of precipitation of ammonium
Centrifuge separation, the scandium fluoride precipitating being enriched with, and the rate of recovery of scandium can achieve 93%.
Embodiment 3
Cyanex272 extractant (two (2,4,4- tri-methyl-amyl) phosphinic acids), HF back extraction
It is 1:20 according to organic solution, the ratio of liquor capacity containing scandium, with containing in the reaction kettle that band is stirred effect
The hexane solution of 4mol/L Cyanex272 extractant extracting scandium from scandium containing 0.01mol/L and 1mol/L hydrochloric acid solution；It will
The organic phase of load scandium is washed with 1mol/L aqueous hydrochloric acid solution, is stripped agent solution according to extractant organic solution, precipitating
Volume ratio (organic solution: aqueous solution volume ratio) be 10:1, by after washing load scandium organic phase with containing the anti-of 9mol/LHF
Extraction agent aqueous solution (water phase) is mixed, and back extraction reaction is carried out, and generates scandium fluoride precipitating；Scandium fluoride precipitating is used into second respectively
Pure and mild water washing, wash temperature are 20 DEG C and 90 DEG C；Scandium fluoride ScF3 is deposited in 90 DEG C of dryings to generate scandium fluoride product, scandium
The rate of recovery can achieve 91%.
Embodiment 4
P204 extractant (di-(2-ethylhexyl)phosphoric acid), HF back extraction
It is 1:1 according to organic solution, the ratio of liquor capacity containing scandium, with containing 1mol/ in the reaction kettle that band is stirred effect
The kerosin of LP507 extractant extracting scandium from scandium containing 0.01mol/L and 0.5mol/L sulfuric acid solution；The organic of scandium will be loaded
It is mutually washed with 0.5mol/L aqueous sulfuric acid, the volume ratio according to extractant organic solution, precipitating back extraction agent solution is (organic
Solution: aqueous solution volume ratio) it is 20:1, by the organic phase of the load scandium after washing and the stripping agent aqueous solution containing 0.8mol/LHF
(water phase) is mixed, and back extraction reaction is carried out, and generates scandium fluoride precipitating；Scandium fluoride precipitating is used into ethyl alcohol and washing respectively
It washs, wash temperature is 40 DEG C and 50 DEG C；Scandium fluoride ScF3 is deposited in 105 DEG C of dryings to generate scandium fluoride product, the recycling of scandium
Rate can achieve 92%.
Embodiment 5
Compared with case study on implementation 1 the difference is that,
Extractant used in it is P507, HF back extraction, by the scandium fluoride ScF of generation3100 DEG C of dryings are deposited in generate fluorine
Change scandium product, wherein the extraction recovery of scandium can achieve 92%.
Case study on implementation 6
Compared with case study on implementation 2 the difference is that,
Extractant used in it is P204, NaF back extraction, by the scandium fluoride ScF of generation3105 DEG C of dryings are deposited in generate
Scandium fluoride product, wherein the extraction recovery of scandium can achieve 95%.
Case study on implementation 7
Compared with case study on implementation 1 the difference is that,
According to extractant organic solution, volume ratio (organic solution, aqueous solution volume ratio) 1:10 of back extraction agent solution, will wash
The organic phase for washing back loading scandium is mixed with the stripping agent aqueous solution (water phase) of the NaF containing 0.2mol/l, reaction temperature 50
DEG C, to carry out back extraction reaction, the scandium fluoride precipitating of generation exports outflow in water phase and from water phase；Unloaded scandium it is organic
It is mutually separated with solution, and returns to extraction step recycling；
By the hydrofluorination scandium precipitating of generation with water phase by isolated by vacuum filtration, the scandium fluoride being enriched with is precipitated；By fluorine
Change after NaF is added in scandium mother liquor of precipitation of ammonium and returns to scandium back extraction processing step use；Scandium fluoride precipitating is used into ethyl alcohol and water washing respectively,
Wash temperature is 30 DEG C and 80 DEG C, to remove the organic matter and water-solubility impurity of adsorption respectively.
By scandium fluoride ScF3100 DEG C of dryings are deposited in generate scandium fluoride product, wherein scandium extraction recovery can achieve
90%.
Case study on implementation 8
It is with the different place of case study on implementation 2,
According to extractant organic solution, volume ratio (organic solution, aqueous solution volume ratio) 1:20 of back extraction agent solution, will wash
The organic phase for washing back loading scandium is mixed with the stripping agent aqueous solution (water phase) of the HF containing 0.05mol/l, reaction temperature 50
DEG C, to carry out back extraction reaction, the scandium fluoride precipitating of generation exports outflow in water phase and from water phase；Unloaded scandium it is organic
It is mutually separated with solution, and returns to extraction step recycling；
By the hydrofluorination scandium precipitating of generation with water phase by isolated by vacuum filtration, the scandium fluoride being enriched with is precipitated；By fluorine
Change after HF is added in scandium mother liquor of precipitation of ammonium and returns to scandium back extraction processing step use；Scandium fluoride precipitating is used into ethyl alcohol and water washing respectively,
Wash temperature is 30 DEG C and 80 DEG C, to remove the organic matter and water-solubility impurity of adsorption respectively.
By scandium fluoride ScF3100 DEG C of dryings are deposited in generate scandium fluoride product, wherein scandium extraction recovery can achieve
88%.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements: by scandium from containing
The extraction of scandium solution, is then added F-To realize, scandium is stripped and is precipitated simultaneously in organic phase, so that scandium ion is directly translated into fluorine
Change scandium precipitating, so that scandium is able to enrichment and separation, while being prepared scandium fluoride product, shortens operating process, subtract
Few back extraction acid neutralizes the consumption of raw materialss such as alkali, water, oxalic acid, reduces operating cost, is conducive to be applied to industrial production.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (16)
1. a kind of method for extracting scandium fluoride, which comprises the following steps:
S1 carries out scandium extraction to inorganic acid solution containing scandium using the organic solvent solution of the extractant containing acidic organo phosphorus, is contained
There is the organic phase of scandium；
S2 carries out carrying out washing treatment to the organic phase containing scandium to remove impurity；
S3 is stripped, liquid liquid point to HF and/or NaF solution is added in the organic phase containing scandium described in removing after impurity
Scandium complex anion solution and unloaded organic phase are obtained from after, and the acid of hydrochloric acid conditioning solution is added into the scandium complex anion solution
Basicity, to generate ScF3It precipitates, obtains ScF after separation of solid and liquid3Precipitating and mother liquor of precipitation of ammonium；
S4, by the ScF3Scandium fluoride product is obtained after washing of precipitate, drying.
2. the method according to claim 1, wherein in the S3, F in HF the and/or NaF solution-Ion with
The ratio between amount of substance of scandium is greater than 3 less than 4.5 in the inorganic acid solution containing scandium.
3. the method according to claim 1, wherein the acidic organo phosphorus extractant is selected from by two (2- ethyls
Hexyl) phosphoric acid, the mono- 2- ethylhexyl of 2- ethylhexyl phosphoric acid and Cyanex272 extractant composition one of group or more
Kind.
4. the method according to claim 1, wherein the organic solvent solution of the extractant containing acidic organo phosphorus
In organic extractant be density be less than water alkanes or at least one of its mixture or arene；
Preferably, the alkanes or its mixture include normal heptane, n-hexane and kerosene；
Preferably, the arene includes benzene and toluene.
5. the method according to claim 3 or 4, which is characterized in that the organic solvent of the extractant containing acidic organo phosphorus
The concentration of the extractant containing acidic organo phosphorus described in solution is 0.01mol/L~4mol/L.
6. the method according to claim 1, wherein the inorganic acid solution containing scandium be sulfuric acid solution containing scandium,
Hydrochloric acid solution or nitric acid solution.
7. the method according to claim 1, wherein the organic solvent solution of the extractant containing acidic organo phosphorus
Volume ratio with the inorganic acid solution containing scandium is (1:20)~(1:1).
8. according to the method described in claim 2, it is characterized in that, the organic solvent solution of the extractant containing acidic organo phosphorus
Volume ratio with HF and/or NaF solution in the S3 is (1:20)~(20:1).
9. the method according to claim 1, wherein the S4 includes: to use ScF described in ethyl alcohol and water washing respectively3
Precipitating.
10. according to the method described in claim 9, being washed with water it is characterized in that, be 20~40 DEG C with the temperature of ethanol washing
Temperature be 50~90 DEG C.
11. the method according to claim 1, wherein in the S2, cleaning solution used in the carrying out washing treatment is
The aqueous hydrochloric acid solution of 0.1~2mol/L or the aqueous sulfuric acid of 0.1~1mol/L.
12. the method according to claim 1, wherein HF and/or NaF is added in the mother liquor of precipitation of ammonium in the S3
It returns to back extraction processing step afterwards to use, the zero load organic phase returns to scandium extraction processing step in S1 and uses.
13. the method according to claim 1, wherein the mixing in scandium extraction and back extraction processing uses
Mechanical mixture stirring or ultrasonic wave mixing are to accelerate extent of reaction.
14. the method according to claim 1, wherein the reaction temperature of the back extraction is 20~70 DEG C, preferably
It is 25~45 DEG C.
15. the method according to claim 1, wherein there is the extractant containing acidic organo phosphorus in the S1
It is small that the ratio between acidic organo phosphorus extractant described in solvent solution and the amount of substance of scandium in the inorganic acid solution containing scandium are greater than 3
In 20.
16. the method according to claim 1, wherein scandium fluoride is precipitated drying to generate fluorination in the S4
The temperature of scandium product is 90~105 DEG C.
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| CN201811143112.7A CN109179479A (en) | 2018-09-28 | 2018-09-28 | The method for extracting scandium fluoride |
| PCT/CN2019/108710 WO2020063913A1 (en) | 2018-09-28 | 2019-09-27 | Preparation method for scandium fluoride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020063913A1 (en) * | 2018-09-28 | 2020-04-02 | 中国恩菲工程技术有限公司 | Preparation method for scandium fluoride |
| CN115872436A (en) * | 2022-12-30 | 2023-03-31 | 河南荣佳钪钒科技有限公司 | Scandium fluoride wet preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020063913A1 (en) * | 2018-09-28 | 2020-04-02 | 中国恩菲工程技术有限公司 | Preparation method for scandium fluoride |
| CN115872436A (en) * | 2022-12-30 | 2023-03-31 | 河南荣佳钪钒科技有限公司 | Scandium fluoride wet preparation method |
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Application publication date: 20190111 |