CN116282090A - Method for separating beryllium from beryllium hydroxide containing impurities by adopting chlorination system and application of method - Google Patents
Method for separating beryllium from beryllium hydroxide containing impurities by adopting chlorination system and application of method Download PDFInfo
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- CN116282090A CN116282090A CN202310151712.2A CN202310151712A CN116282090A CN 116282090 A CN116282090 A CN 116282090A CN 202310151712 A CN202310151712 A CN 202310151712A CN 116282090 A CN116282090 A CN 116282090A
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- 229910052790 beryllium Inorganic materials 0.000 title claims abstract description 112
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- WPJWIROQQFWMMK-UHFFFAOYSA-L beryllium dihydroxide Chemical compound [Be+2].[OH-].[OH-] WPJWIROQQFWMMK-UHFFFAOYSA-L 0.000 title claims abstract description 82
- 229910001865 beryllium hydroxide Inorganic materials 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 79
- 239000012535 impurity Substances 0.000 title claims abstract description 51
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000012074 organic phase Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims description 177
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 70
- 238000000605 extraction Methods 0.000 claims description 59
- 229910052742 iron Inorganic materials 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 16
- -1 iron ions Chemical class 0.000 claims description 16
- 239000003350 kerosene Substances 0.000 claims description 16
- 229910001423 beryllium ion Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 10
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 8
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 5
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims description 4
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000012747 synergistic agent Substances 0.000 claims description 4
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 2
- 229910001447 ferric ion Inorganic materials 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 13
- 238000011084 recovery Methods 0.000 abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 48
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- KQHXBDOEECKORE-UHFFFAOYSA-L beryllium sulfate Chemical compound [Be+2].[O-]S([O-])(=O)=O KQHXBDOEECKORE-UHFFFAOYSA-L 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- JZKFIPKXQBZXMW-UHFFFAOYSA-L beryllium difluoride Chemical compound F[Be]F JZKFIPKXQBZXMW-UHFFFAOYSA-L 0.000 description 1
- 229910001633 beryllium fluoride Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000004334 fluoridation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 125000005608 naphthenic acid group Chemical group 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C01F3/00—Compounds of beryllium
- C01F3/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for separating beryllium from beryllium hydroxide containing impurities by adopting a chlorination system and application thereof, wherein the method comprises the following steps: dissolving the beryllium hydroxide with hydrochloric acid solution to obtain hydrochloric acid acidolysis solution, and extracting with extractant to obtain loaded organic phase and beryllium-rich raffinate. The method provided by the invention can separate the beryllium in the impurity-containing beryllium hydroxide from impurities to obtain the beryllium-rich raffinate, so that the impurity-containing beryllium hydroxide is purified, and the method has the advantages of more sufficient separation of the beryllium and the impurities, higher recovery rate of the beryllium in the impurity-containing beryllium hydroxide, simple process and easiness in large-scale popularization and use.
Description
Technical Field
The invention belongs to the technical field of beryllium hydroxide purification, relates to a method for separating beryllium from mixed beryllium hydroxide by adopting a chlorination system, and particularly relates to a method for separating beryllium from mixed beryllium hydroxide by adopting a chlorination system and application of the method.
Background
Beryllium is an important strategic metal element and is widely applied to the fields of nuclear industry, aerospace, precise instruments and meters, military high and new technologies and the like. Currently, very few countries in the world have complete systems for large-scale exploitation, extraction of metallurgy and metal processing. The smelting method of beryllium mainly comprises a sulfuric acid method, a fluoridation method, a sulfuric acid-hydrolysis method and a sulfuric acid-extraction method, and the obtained intermediate product is beryllium hydroxide. Industrial-grade beryllium hydroxide contains a plurality of metal impurities (Fe, al, ca, mg, zn, mn, cr) and rare earth element ions, which are not beneficial to improving the purity of beryllium fluoride and beryllium beads in the subsequent process, so how to refine the beryllium hydroxide is the research focus of the technicians in the field.
The beryllium hydroxide refining and purifying process has few reports, iron is one of main impurity elements of industrial-grade beryllium hydroxide, and most of iron removal methods in the beryllium hydroxide refining processes disclosed in the literature and patent published at home and abroad at present are separated by chemical methods, and mainly comprise the following steps: 1) The beryllium sulfate crystallization method adopts sulfuric acid to dissolve beryllium hydroxide, and excessive ammonium sulfate is added to repeatedly crystallize aluminum alum, thus obtaining high-purity beryllium sulfate crystals; 2) Precipitation methods, which are divided into an acidic precipitation method and an alkaline precipitation method, wherein the alkaline precipitation method, such as patent CN111422890a and CN105585034a, discloses dissolving beryllium hydroxide by sodium hydroxide, adjusting pH value for hydrolysis, and then washing and precipitating to obtain higher-purity beryllium hydroxide; wherein, an acid precipitation method, for example, patent CN103663506A discloses that after beryllium hydroxide is dissolved by sulfuric acid, the mixture is mixed with animal glue and evaporated to dryness, and then impurities such as silicon and the like are removed, the filtrate is shielded by using an EDTA complex precipitation method, and iron and part of aluminum ions are removed, so as to obtain refined beryllium hydroxide; 3) Solvent extraction methods, such as those described in CN103818937a and CN102851502a, disclose the purification of a multi-beryllium solution by extraction of beryllium, involving mainly phosphoric acid type extractants and naphthenic acids. However, in the three methods, the beryllium sulfate crystallization method has poor impurity removal effect, is troublesome to operate and is difficult to realize in a process; the precipitation method cannot deeply remove impurities such as iron and the like; in the existing solvent extraction method, the extraction stage number is more, the operation is difficult, and the selectivity of the extractant to beryllium iron is poor, so that iron impurities are difficult to remove.
The existing beryllium hydroxide purification methods have certain defects, and have the problems of poor impurity removal effect, complex process and difficult operation. Therefore, it is important to develop a new method for separating beryllium from beryllium hydroxide with impurities by using a chlorination system and application thereof.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for separating beryllium in the beryllium hydroxide with impurities by adopting a chlorination system and application thereof.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for separating beryllium from contaminated beryllium hydroxide using a chlorination system, the method comprising:
dissolving the beryllium hydroxide with hydrochloric acid solution to obtain hydrochloric acid acidolysis solution, and extracting with extractant solution to obtain loaded organic phase and beryllium-rich raffinate.
The method provided by the invention can separate the beryllium in the impurity-containing beryllium hydroxide from impurities to obtain the beryllium-rich raffinate, so that the impurity-containing beryllium hydroxide is purified, and the method has the advantages of more sufficient separation of the beryllium and the impurities, higher recovery rate of the beryllium in the impurity-containing beryllium hydroxide, simple process and easiness in large-scale popularization and use.
The concentration of the hydrochloric acid solution is preferably 10% to 38%, and may be, for example, 12%, 15%, 17%, 20%, 22%, 25%, 27%, 30%, 32%, 35% or 38%, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the dissolution is performed with heating.
Preferably, the heating temperature is 20-90 ℃ and the heating time is 5-30 min.
The heating temperature of the present invention is 20 to 90℃and may be, for example, 20℃25℃30℃35℃40℃45℃50℃55℃60℃65℃70℃75℃80℃85℃or 90℃but is not limited to the values listed, and other values not listed in the range are equally applicable.
The heating time in the present invention is 5 to 30 minutes, and may be, for example, 5 minutes, 10 minutes, 15 minutes, 20 minutes, 25 minutes or 30 minutes, but is not limited to the values listed, and other values not listed in the range are applicable.
Preferably, the mass ratio of the hydrochloric acid solution to the mixed beryllium hydroxide in the dissolution process is (1.0-5.0): 1, for example, but not limited to, the listed values, other non-listed values in the range of values are equally applicable, and the mass ratio may be 1.5:1, 1.6:1, 1.7:1, 1.8:1, 1.9:1, 2:1, 2.1:1, 2.2:1, 2.3:1, 2.4:1, 2.5:1, 3:1, 3.5:1, 4:1, 4.5:1 or 5:1.
Preferably, the mass fraction of beryllium hydroxide in the impurity-containing beryllium hydroxide is 80-98 wt%, for example, 80wt%, 80.5wt%, 81wt%, 81.5wt%, 82wt%, 82.5wt%, 830wt%, 83.5wt%, 84wt%, 84.5wt%, 85wt%, 88wt%, 90wt%, 92wt%, 94wt%, 96wt% or 98wt%, but is not limited to the recited values, and other non-recited values in the range of values are equally applicable, and the remainder is impurities.
Preferably, the impurity includes iron, and the mass fraction of iron in the impurity-containing beryllium hydroxide is 0.001 to 0.06wt%, and may be, for example, 0.001wt%, 0.005wt%, 0.01wt%, 0.02wt%, 0.001wt%, 0.03wt%, 0.035wt%, 0.04wt%, 0.045wt%, 0.05wt%, 0.055wt%, or 0.06wt%, but is not limited to the recited values, and other non-recited values in the range of values are equally applicable.
The impurities of the present invention also include sulfate impurities.
The mixed beryllium hydroxide disclosed by the invention comprises industrial beryllium hydroxide.
The industrial beryllium hydroxide is in powder form.
The concentration of beryllium ions in the acid hydrolysis solution of hydrochloric acid is preferably 20 to 40g/L, and may be, for example, 20g/L, 25g/L, 30g/L, 35g/L, 35.5g/L, 36g/L, 37g/L, 38.5g/L, 39g/L, 39.5g/L or 40g/L, but is not limited to the values listed, and other values not listed in the range of values are equally applicable.
The concentration of iron ions in the acid hydrolysis solution of hydrochloric acid is preferably 0.01 to 0.1g/L, and may be, for example, 0.01g/L, 0.03g/L, 0.05g/L, 0.07g/L, 0.075g/L, 0.08g/L, 0.085g/L, 0.09g/L, 0.095g/L, or 0.1g/L, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned values are equally applicable.
Preferably, between the dissolving and extracting, further comprises: the solution is diluted and the pH of the hydrochloric acid acidolysis solution is adjusted to 0 to 3.5, for example, 0, 0.2, 0.4, 0.6, 0.8, 1, 1.2, 1.4, 1.6, 1.8, 2, 2.2, 2.4, 2.6, 2.8, 3, 3.5, to obtain the solution to be extracted.
Preferably, the conditioning comprises adding sodium hydroxide solution.
The concentration of the sodium hydroxide solution is preferably 5 to 10mol/L, and may be, for example, 5mol/L, 6mol/L, 7mol/L, 8mol/L, 9mol/L or 10mol/L, but is not limited to the recited values, and other values not recited in the range of the recited values are equally applicable.
Preferably, the concentration of beryllium ions in the solution to be extracted is 0.5-40 g/L, for example, but not limited to the listed values, and other non-listed values in the range of the values are equally applicable.
Preferably, the concentration of the ferric ions in the solution to be extracted is 0.001-0.1 g/L, for example, but not limited to the listed values, the values are also applicable within the range of the values, and the concentration is 0.001g/L, 0.002g/L, 0.003g/L, 0.005g/L, 0.007g/L, 0.01g/L, 0.02g/L, 0.03g/L, 0.04g/L, 0.05g/L, 0.06g/L, 0.07g/L, 0.08g/L, 0.09g/L or 0.1g/L.
Preferably, the volume ratio of the extractant solution to the liquid to be extracted is 0.5-5:1, for example, it may be 0.5:1, 0.7:1, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 3.5:1, 4:1, 4.5:1 or 5:1, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the extraction temperature is 20-30 ℃ and the extraction time is 5-15 min.
The extraction temperature in the present invention is 20 to 30℃and may be, for example, 20℃21℃22℃23℃24℃25℃26℃27℃28℃29℃or 30℃but is not limited to the values listed, and other values not listed in the range are equally applicable.
The extraction time in the present invention is 5 to 15 minutes, and may be, for example, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes or 15 minutes, but is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
Preferably, the extractant in the extractant solution comprises TBP, P507, cyanex272 or naphthenic acid.
Preferably, the solvent in the extractant solution comprises any one or a combination of at least two of kerosene, cyclohexane, toluene, xylene, carbon tetrachloride, or MIBK, typically but not limited to a combination of kerosene and cyclohexane, a combination of cyclohexane and toluene, a combination of xylene and carbon tetrachloride, a combination of carbon tetrachloride and MIBK, or a combination of kerosene, cyclohexane, and toluene.
Preferably, the extractant solution further comprises a co-extractant.
Preferably, the co-extractant comprises any one or a combination of at least two of TBP, isooctanol, n-pentanol, n-octanol, isooctanoic acid, or isopropanol, typically but not limited to combinations comprising TBP and isooctanol, n-pentanol and n-octanol, n-octanol and isooctanoic acid, isooctanoic acid and isopropanol, TBP, isooctanol and n-pentanol, or isooctanol, n-pentanol, n-octanol and isooctanoic acid.
The mass ratio of the extractant to the synergistic agent in the invention is 1 (0.2-0.5), for example, 1:0.2, 1:0.25, 1:0.3, 1:0.35, 1:0.4, 1:0.45 or 1:0.5, but the invention is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the sum of the mass percentages of the extractant and the synergistic agent is 10-60 wt% and the mass percentage of the solvent is 40-90 wt% based on the mass percentage of the extractant solution.
The total mass fraction of the extractant and the co-extractant in the present invention is 10 to 60wt%, for example, 10wt%, 12wt%, 15wt%, 17wt%, 20wt%, 22wt%, 25wt%, 27wt%, 30wt%, 32wt%, 35wt%, 37wt%, 40wt%, 45wt%, 50wt%, 55wt% or 60wt%, but not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
The mass fraction of the solvent according to the present invention is 40 to 90wt%, for example, 40wt%, 45wt%, 560wt%, 55wt%, 60wt%, 62wt%, 65wt%, 67wt%, 70wt%, 72wt%, 75wt%, 77wt%, 80wt%, 82wt%, 85wt%, 87wt% or 90wt%, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the extraction temperature is 20-30 ℃ and the extraction time is 10-20 min.
The extraction temperature of the present invention may be 20 to 30℃and may be, for example, 20℃and 21℃and 22℃and 23℃and 24℃and 25℃and 26℃and 27℃and 28℃and 29℃or 30℃and is not limited to the values listed, but other values not listed in the range are applicable.
The extraction time of the present invention is 10 to 20 minutes, and may be, for example, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes or 20 minutes, but is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
Preferably, the method further comprises a first stripping after the extraction, the first stripping comprising: and back-extracting the loaded organic phase by using an acid solution to obtain a beryllium-rich organic solution and an impurity ion-rich aqueous solution.
The first back extraction is used for extracting impurity ions in the loaded organic phase obtained after extraction, and beryllium-rich organic solution is obtained, so that further extraction and separation of beryllium are realized.
The concentration of the acid solution is preferably 0.5 to 6mol/L, and may be, for example, 0.5mol/L, 1mol/L, 1.5mol/L, 2mol/L, 2.5mol/L, 3mol/L, 3.5mol/L, 4mol/L, 4.5mol/L, 5mol/L, 5.5mol/L, or 6mol/L, but is not limited to the recited values, and other values not recited in the range of the values are equally applicable.
Preferably, the acid solution comprises a hydrochloric acid solution and/or a sulfuric acid solution.
Preferably, the volume ratio of the acid solution to the loaded organic phase is 1 (0.5-5), for example, it may be 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:0.5, 1:4.5 or 1:5, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the temperature of the first back extraction is 20-30 ℃ and the time is 5-20 min.
The temperature of the first stripping in the present invention may be 20 to 30℃and may be, for example, 20℃and 21℃and 22℃and 23℃and 24℃and 25℃and 26℃and 27℃and 28℃and 29℃or 30℃but is not limited to the values listed, and other values not listed in the range are equally applicable.
The time of the first back extraction in the present invention is 5 to 20min, for example, 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min or 20min, but the present invention is not limited to the recited values, and other non-recited values in the range of the values are applicable.
Preferably, the method further comprises a second stripping after the first stripping, the second stripping comprising: and back-extracting the beryllium-rich organic solution by using alkali solution to obtain an organic solution and a beryllium-rich aqueous solution.
The second back extraction is used for extracting the beryllium in the beryllium-rich organic solution obtained after the first back extraction, so that a beryllium-rich aqueous solution is obtained, and further extraction and separation of the beryllium are realized.
The concentration of the alkali solution is preferably 1 to 6mol/L, and may be, for example, 1mol/L, 2mol/L, 3mol/L, 4mol/L, 5mol/L, or 6mol/L, but is not limited to the recited values, and other values not recited in the range of the recited values are equally applicable.
Preferably, the alkaline solution comprises any one or a combination of at least two of a sodium hydroxide solution, a calcium hydroxide solution, or a potassium hydroxide solution, typically but not limited to a combination of a sodium hydroxide solution and a calcium hydroxide solution, a combination of a calcium hydroxide solution and a potassium hydroxide solution, or a combination of a sodium hydroxide solution, a calcium hydroxide solution, and a potassium hydroxide solution.
Preferably, the volume ratio of the alkaline solution to the beryllium-rich organic solution is 1 (0.5-5), for example, 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5 or 1:5, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the temperature of the second back extraction is 20-30 ℃ and the time is 5-20 min.
The temperature of the second stripping in the present invention is 20 to 30 ℃, and may be, for example, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃ or 30 ℃, but is not limited to the values recited, and other values not recited in the range are equally applicable.
The second stripping time of the present invention is 5 to 20 minutes, for example, 5 minutes, 7 minutes, 10 minutes, 12 minutes, 15 minutes, 17 minutes or 20 minutes, but the present invention is not limited to the recited values, and other non-recited values within the range are equally applicable.
As a preferred embodiment of the method according to the invention, the method comprises:
(1) Dissolving mixed beryllium hydroxide in hydrochloric acid solution with the concentration of 10% -38%, wherein the mass fraction of beryllium hydroxide in the mixed beryllium hydroxide is 80-98 wt%, the mass fraction of iron is 0.001-0.06 wt%, the mass ratio of the hydrochloric acid solution to the mixed beryllium hydroxide is (1.0-5.0): 1, and heating the mixture at 20-90 ℃ for 5-30 min during dissolving to obtain hydrochloric acid hydrolysis solution with the concentration of beryllium ions of 20-40 g/L and the concentration of iron ions of 0.001-0.1 g/L;
(2) Diluting the solution and regulating the pH value of the hydrochloric acid acidolysis solution obtained in the step (1) to 0-3.5 to obtain a solution to be extracted, wherein the concentration of beryllium ions is 0.5-40 g/L and the concentration of iron ions is 0.001-0.1 g/L;
(3) Extracting the liquid to be extracted obtained in the step (2) by using an extractant solution, wherein the extractant solution comprises an extractant, a co-extractant and a solvent, the sum of the mass fractions of the extractant and the co-extractant is 10-60 wt% based on the mass percentage of the extractant solution, the mass fraction of the solvent is 40-90 wt%, and the volume ratio of the extractant solution to the liquid to be extracted is 0.5-5:1, so as to obtain a loaded organic phase and beryllium-rich raffinate;
(4) Carrying out back extraction on the loaded organic phase obtained in the step (3) by using an acid solution with the concentration of 0.5-6 mol/L, wherein the volume ratio of the acid solution to the loaded organic phase is 1 (0.5-5), so as to obtain a beryllium-rich organic solution and an impurity ion-rich aqueous solution;
(5) Back-extracting the beryllium-rich organic solution obtained in the step (4) by using an alkali solution with the concentration of 1-6 mol/L, wherein the volume ratio of the alkali solution to the beryllium-rich organic solution is 1 (0.5-5), so as to obtain the organic solution and the beryllium-rich aqueous solution.
The method comprises the steps of obtaining beryllium-rich raffinate after one-step extraction, realizing beryllium extraction and separation in the beryllium hydroxide containing impurities, carrying out primary back extraction on a loaded organic phase to extract and separate impurity ions in the loaded organic phase to obtain a beryllium-rich organic solution, carrying out secondary back extraction on the beryllium-rich organic solution, and extracting beryllium in the beryllium-rich organic solution to obtain a beryllium-rich aqueous solution; the beryllium extract obtained by the method is a beryllium-rich raffinate and a beryllium-rich aqueous solution.
In a second aspect, the invention provides the use of the method of the first aspect for purification of beryllium hydroxide.
Compared with the prior art, the invention has the following beneficial effects:
the method provided by the invention can separate the beryllium in the impurity-containing beryllium hydroxide from impurities to obtain the beryllium-rich raffinate, so that the impurity-containing beryllium hydroxide is purified, and the method has the advantages of more sufficient separation of the beryllium and the impurities, higher recovery rate of the beryllium in the impurity-containing beryllium hydroxide, simple process and easiness in large-scale popularization and use.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a method for separating beryllium in industrial beryllium hydroxide by adopting a chlorination system, which comprises the following steps:
(1) Dissolving industrial beryllium hydroxide by using a hydrochloric acid solution with the concentration of 37.5%, wherein the mass ratio of the hydrochloric acid solution to the industrial beryllium hydroxide is 2.2:1, and heating at 30 ℃ for 10min during dissolving to obtain hydrochloric acid acidolysis solution of beryllium hydroxide with the concentration of beryllium ions of 30g/L and the concentration of iron ions of 0.7 g/L;
(2) Diluting the solution, adding 6mol/L sodium hydroxide solution to adjust the pH value of the hydrochloric acid acidolysis solution obtained in the step (1) to 3.5, and obtaining a solution to be extracted, wherein the concentration of beryllium ions is 11g/L and the concentration of iron ions is 0.025 g/L;
(3) Extracting the liquid to be extracted obtained in the step (2) by using an extractant solution, wherein the extractant solution comprises Cyanex272 and kerosene, the mass fraction of Cyanex272 is 40wt% and the mass fraction of kerosene is 60wt% based on the mass of the extractant solution, the extractant solution is a solution which is saponified by 10mol/L sodium hydroxide solution and 40%, and the volume ratio of the extractant solution to the liquid to be extracted is 1:1, so as to obtain a loaded organic phase and beryllium-rich raffinate;
(4) Carrying out back extraction on the loaded organic phase obtained in the step (3) by using a sulfuric acid solution with the concentration of 0.5mol/L, wherein the volume ratio of the hydrochloric acid solution to the loaded organic phase is 1:0.5, so as to obtain a beryllium-rich organic solution and an impurity ion-rich aqueous solution;
(5) And (3) back-extracting the beryllium-rich organic solution obtained in the step (4) by using a sodium hydroxide solution with the concentration of 1mol/L, wherein the volume ratio of the sodium hydroxide solution to the beryllium-rich organic solution is 1:0.5, and thus the organic solution and the beryllium-rich aqueous solution are obtained.
Example 2
The embodiment provides a method for separating beryllium in industrial beryllium hydroxide by adopting a chlorination system, which comprises the following steps:
(1) Dissolving industrial beryllium hydroxide by using a hydrochloric acid solution with the concentration of 10%, wherein the mass ratio of the hydrochloric acid solution to the industrial beryllium hydroxide is 5:1, and heating at 90 ℃ for 5min during dissolving to obtain beryllium hydroxide hydrochloric acid acidolysis solution with the concentration of beryllium ions of 40g/L and the concentration of iron ions of 0.1g/L;
(2) Diluting the solution, adding 10mol/L sodium hydroxide to adjust the pH value of the hydrochloric acid acidolysis solution obtained in the step (1) to 0, and obtaining a solution to be extracted, wherein the concentration of beryllium ions is 0.5g/L and the concentration of iron ions is 0.001 g/L;
(3) Extracting the liquid to be extracted obtained in the step (2) by using an extractant solution, wherein the extractant solution comprises naphthenic acid, isooctanol and kerosene, the mass fraction of the naphthenic acid is 20wt%, the mass fraction of the isooctanol is 20wt%, the mass fraction of the kerosene is 60wt%, and the extractant solution is a solution obtained by saponifying 40% of 10mol/L sodium hydroxide solution; the volume ratio of the extractant solution to the liquid to be extracted is 0.5:1, and a loaded organic phase and beryllium-rich raffinate are obtained;
(4) Carrying out back extraction on the loaded organic phase obtained in the step (3) by using a hydrochloric acid solution with the concentration of 6mol/L, wherein the volume ratio of the hydrochloric acid solution to the loaded organic phase is 1:5, so as to obtain a beryllium-rich organic solution and an impurity ion-rich aqueous solution;
(5) And (3) back-extracting the beryllium-rich organic solution obtained in the step (4) by using a sodium hydroxide solution with the concentration of 6mol/L, wherein the volume ratio of the sodium hydroxide solution to the beryllium-rich organic solution is 1:5, and thus the organic solution and the beryllium-rich aqueous solution are obtained.
Example 3
The embodiment provides a method for separating beryllium in industrial beryllium hydroxide by adopting a chlorination system, which comprises the following steps:
(1) Dissolving industrial beryllium hydroxide by using a hydrochloric acid solution with the concentration of 38%, wherein the mass ratio of the hydrochloric acid solution to the industrial beryllium hydroxide is 1:1, and heating at 20 ℃ for 30min during dissolving to obtain a hydrochloric acid acidolysis solution of beryllium hydroxide with the concentration of 20g/L beryllium ions and the concentration of 0.001g/L iron ions;
(2) Diluting the solution, adding 10mol/L sodium hydroxide solution to adjust the pH value of the hydrochloric acid acidolysis solution obtained in the step (1) to 1, and obtaining a solution to be extracted, wherein the concentration of beryllium ions is 36g/L and the concentration of iron ions is 0.1g/L;
(3) Extracting the liquid to be extracted obtained in the step (2) by using an extractant solution, wherein the extractant solution comprises P507, TBP and kerosene, the mass fraction of the P507 is 30wt%, the mass fraction of the TBP is 30wt%, the mass fraction of the kerosene is 40wt%, the extractant solution is a solution which is saponified by 10mol/L sodium hydroxide solution and is 40%, and the volume ratio of the extractant solution to the liquid to be extracted is 5:1, so that the loaded organic phase loaded with iron and the beryllium-rich raffinate are obtained.
Example 4
The embodiment provides a method for separating beryllium in industrial beryllium hydroxide by adopting a chlorination system, which comprises the following steps:
(1) Dissolving industrial beryllium hydroxide hydrochloric acid solution and industrial beryllium hydroxide by using hydrochloric acid solution with the concentration of 37.5% in a mass ratio of 2:1, and heating at 300 ℃ for 10min during dissolving to obtain hydrochloric acid acidolysis solution with the concentration of beryllium ions of 38g/L and the concentration of iron ions of 0.07 g/L;
(2) Extracting the liquid to be extracted obtained in the step (1) by using an extractant solution, wherein the extractant solution comprises TBP and kerosene, the mass fraction of the TBP is 10wt% and the mass fraction of the kerosene is 90wt% based on the mass of the extractant solution, and the volume ratio of the extractant solution to the liquid to be extracted is 1:1, so that a loaded organic phase loaded with iron and a beryllium-rich raffinate are obtained.
Example 5
The present example provides a method for separating beryllium from industrial beryllium hydroxide using a chlorination system, the remainder being the same as example 4 except that the mass fraction of TBP is 2wt% and the mass fraction of kerosene is 98wt% based on the mass of the extractant solution.
Example 6
The present example provides a method for separating beryllium from industrial beryllium hydroxide using a chlorination system, the remainder being the same as example 4 except that the mass fraction of TBP is 70wt% and the mass fraction of kerosene is 30wt% based on the mass of the extractant solution.
Example 7
The present example provides a method for separating beryllium from industrial beryllium hydroxide using a chlorination system, the remainder being the same as in example 4 except that the volume ratio of extractant solution to liquid to be extracted in step (3) is 0.3:1.
Example 8
The present example provides a method for separating beryllium from industrial beryllium hydroxide using a chlorination system, the remainder being the same as in example 4 except that the volume ratio of the extractant solution to the liquid to be extracted in step (3) is 6:1.
Example 9
The present example provides a method for separating beryllium from industrial beryllium hydroxide using a chlorination system, the remainder being the same as in example 3 except that the mass fraction of TBP is 2wt%, the mass fraction of P507 is 2wt%, and the mass fraction of kerosene is 96wt% based on the mass of the extractant solution.
Example 10
The present example provides a method for separating beryllium from industrial beryllium hydroxide using a chlorination system, the remainder being the same as in example 3 except that the mass fraction of TBP is 35wt%, the mass fraction of P507 is 35wt%, and the mass fraction of kerosene is 30wt% based on the mass of the extractant solution.
The beryllium-rich raffinate, the beryllium-rich organic solution and the beryllium-rich aqueous solution obtained in the methods of the above examples and comparative examples were tested to obtain the beryllium extraction rate and the iron extraction rate data in the extraction process in step (3) as shown in table 1, the beryllium extraction rate and the iron extraction rate in the back extraction process in step (4) as shown in table 1, and the beryllium extraction rate and the iron extraction rate in the back extraction process in step (5) as shown in table 1.
TABLE 1
From table 1:
(1) In the method for separating beryllium in industrial beryllium hydroxide by adopting a chlorination system in the embodiments 1-2, the extraction rate of beryllium is higher, the extraction rate of iron is lower, and the beryllium in the mixed beryllium hydroxide can be separated from the iron by extraction; the extraction rate of beryllium is lower and the extraction rate of iron is higher in the back extraction process of the loaded organic phase obtained after extraction, so that the separation of beryllium and iron in the loaded organic phase is successfully realized; the extraction rate of beryllium is higher and the extraction rate of iron is lower in the back extraction process of the beryllium-rich organic solution obtained after back extraction, so that the beryllium is successfully extracted and separated from the beryllium-rich organic solution;
(2) As can be seen from the comparison of examples 4, 5 and 6 and examples 3 and 9 and 10, the sum of the mass percentages of the extractant and the co-extractant affects the extraction and separation effect of beryllium based on the mass percentage of the extractant solution; when the concentration of the extractant is low, the extraction capacity of the extractant to iron is insufficient, and when the concentration of the extractant is too high, beryllium and iron are co-extracted, and beryllium and iron cannot be separated in one step. When the sum of the mass fractions of the extractant and the synergistic extractant is too low, the extraction capacity of the extractant solution is reduced, so that the selectivity in the extraction process is reduced, and the separation of beryllium and iron is difficult to realize; when the sum of the mass fractions of the extractant and the synergistic extractant is too high, the extraction capacity of the extractant solution is too strong, so that the selectivity in the extraction process is reduced, and the separation of beryllium and iron is difficult to realize;
(4) As can be seen from the comparison of the example 4 with the examples 7 and 8, the volume ratio of the extractant solution to the liquid to be extracted affects the extraction and separation effect of beryllium; when the volume ratio of the extractant solution to the liquid to be extracted is low, the selectivity in the extraction process is reduced, and the separation of beryllium and iron is difficult to realize;
in conclusion, the method provided by the invention can separate the beryllium in the impurity-containing beryllium hydroxide from the impurities to obtain the beryllium-rich raffinate, so that the impurity-containing beryllium hydroxide is purified, and the method has the advantages of more sufficient separation of the beryllium from the impurities, higher recovery rate of the beryllium in the impurity-containing beryllium hydroxide, simple process and easiness in large-scale popularization and use.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that fall within the technical scope of the present invention disclosed herein are within the scope of the present invention.
Claims (10)
1. A method for separating beryllium from contaminated beryllium hydroxide by using a chlorination system, the method comprising:
dissolving the beryllium hydroxide with hydrochloric acid solution to obtain hydrochloric acid acidolysis solution, and extracting with extractant solution to obtain loaded organic phase and beryllium-rich raffinate.
2. The method of claim 1, wherein the concentration of the hydrochloric acid solution is 10% to 38%;
preferably, the dissolution is performed with heating;
preferably, the heating temperature is 20-90 ℃ and the heating time is 5-30 min;
preferably, the mass ratio of the hydrochloric acid solution to the mixed beryllium hydroxide in the dissolution process is (1.0-5.0): 1.
3. The method according to claim 1 or 2, wherein the mass fraction of beryllium hydroxide in the impurity-containing beryllium hydroxide is 80-98 wt%, the remainder being impurities;
preferably, the impurity includes iron, and the mass fraction of iron in the impurity-containing beryllium hydroxide is 0.001-0.06 wt%.
4. A process according to any one of claims 1 to 3, wherein the concentration of beryllium ions in the hydrochloric acid acidolysis solution is 20 to 40g/L;
preferably, the concentration of iron ions in the hydrochloric acid acidolysis solution is 0.01-0.1 g/L.
5. The method according to any one of claims 1 to 4, wherein between the dissolving and the extracting further comprises: diluting the solution and regulating the pH value of the hydrochloric acid acidolysis solution to 0-3.5 to obtain a solution to be extracted;
preferably, the concentration of beryllium ions in the liquid to be extracted is 0.5-40 g/L;
preferably, the concentration of the ferric ions in the liquid to be extracted is 0.001-0.1 g/L;
preferably, the volume ratio of the extractant solution to the liquid to be extracted is 0.5-5:1.
6. The method of any one of claims 1 to 5, wherein the extractant in the extractant solution comprises any one of TBP, P507, cyanex272 or naphthenic acid;
preferably, the solvent in the extractant solution comprises any one or a combination of at least two of kerosene, cyclohexane, toluene, xylene, carbon tetrachloride or MIBK;
preferably, the extractant solution further comprises a co-extractant;
preferably, the synergistic agent comprises any one or a combination of at least two of TBP, isooctanol, n-amyl alcohol, n-octanol, isooctanoic acid and isopropanol;
preferably, the sum of the mass percentages of the extractant and the synergistic agent is 10-60 wt% and the mass percentage of the solvent is 40-90 wt% based on the mass percentage of the extractant solution.
7. The process according to any one of claims 1 to 6, further comprising a first stripping after the extraction, the first stripping comprising: back-extracting the loaded organic phase by using an acid solution to obtain a beryllium-rich organic solution and an impurity ion-rich aqueous solution;
preferably, the concentration of the acid solution is 0.5-6 mol/L;
preferably, the volume ratio of the acid solution to the loaded organic phase is 1 (0.5-5).
8. The method of claim 7, further comprising a second stripping after the first stripping, the second stripping comprising: back-extracting the beryllium-rich organic solution by using alkali solution to obtain an organic solution and a beryllium-rich aqueous solution;
preferably, the concentration of the alkali solution is 1-6 mol/L;
preferably, the volume ratio of the alkali solution to the beryllium-rich organic solution is 1 (0.5-5).
9. The method according to any one of claims 1 to 8, characterized in that it comprises:
(1) Dissolving mixed beryllium hydroxide in hydrochloric acid solution with the concentration of 10% -38%, wherein the mass fraction of beryllium hydroxide in the mixed beryllium hydroxide is 80-98 wt%, the mass fraction of iron is 0.001-0.06 wt%, the mass ratio of the hydrochloric acid solution to the mixed beryllium hydroxide is (1.0-5.0): 1, and heating the mixture at 20-90 ℃ for 5-30 min during dissolving to obtain hydrochloric acid hydrolysis solution with the concentration of beryllium ions of 20-40 g/L and the concentration of iron ions of 0.001-0.1 g/L;
(2) Diluting the solution and regulating the pH value of the hydrochloric acid acidolysis solution obtained in the step (1) to 0-3.5 to obtain a solution to be extracted, wherein the concentration of beryllium ions is 0.5-40 g/L and the concentration of iron ions is 0.001-0.1 g/L;
(3) Extracting the liquid to be extracted obtained in the step (2) by using an extractant solution, wherein the extractant solution comprises an extractant, a co-extractant and a solvent, the sum of the mass fractions of the extractant and the co-extractant is 10-60 wt% based on the mass percentage of the extractant solution, the mass fraction of the solvent is 40-90 wt%, and the volume ratio of the extractant solution to the liquid to be extracted is 0.5-5:1, so as to obtain a loaded organic phase and beryllium-rich raffinate;
(4) Carrying out back extraction on the loaded organic phase obtained in the step (3) by using an acid solution with the concentration of 0.5-6 mol/L, wherein the volume ratio of the acid solution to the loaded organic phase is 1 (0.5-5), so as to obtain a beryllium-rich organic solution and an impurity ion-rich aqueous solution;
(5) Back-extracting the beryllium-rich organic solution obtained in the step (4) by using an alkali solution with the concentration of 1-6 mol/L, wherein the volume ratio of the alkali solution to the beryllium-rich organic solution is 1 (0.5-5), so as to obtain the organic solution and the beryllium-rich aqueous solution.
10. Use of the method according to any one of claims 1 to 9 for the purification of beryllium hydroxide.
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