CN108085491B - A kind of method that neutrality phosphine extractant is used for extraction and separation thorium - Google Patents
A kind of method that neutrality phosphine extractant is used for extraction and separation thorium Download PDFInfo
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- CN108085491B CN108085491B CN201611110454.XA CN201611110454A CN108085491B CN 108085491 B CN108085491 B CN 108085491B CN 201611110454 A CN201611110454 A CN 201611110454A CN 108085491 B CN108085491 B CN 108085491B
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- diphenyl
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- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 title claims abstract description 124
- 229910052776 Thorium Inorganic materials 0.000 title claims abstract description 124
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000605 extraction Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000000926 separation method Methods 0.000 title claims abstract description 39
- 229910000073 phosphorus hydride Inorganic materials 0.000 title claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 20
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 claims abstract description 12
- 239000003085 diluting agent Substances 0.000 claims abstract description 10
- -1 diphenyl isopentylphosphonate Chemical compound 0.000 claims description 35
- 230000007935 neutral effect Effects 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 24
- 239000012074 organic phase Substances 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 8
- CINZJKLTOKJRGR-UHFFFAOYSA-N [octyl(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(CCCCCCCC)OC1=CC=CC=C1 CINZJKLTOKJRGR-UHFFFAOYSA-N 0.000 claims description 4
- ISGDWKAQZUGYOZ-UHFFFAOYSA-N [tert-butyl(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(C(C)(C)C)OC1=CC=CC=C1 ISGDWKAQZUGYOZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000010290 biphenyl Nutrition 0.000 claims description 4
- 239000004305 biphenyl Substances 0.000 claims description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- IKZDQUQZLWJOPL-UHFFFAOYSA-N [2-methylpropyl(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(CC(C)C)OC1=CC=CC=C1 IKZDQUQZLWJOPL-UHFFFAOYSA-N 0.000 claims description 2
- LKMDHQMGVTVIRI-UHFFFAOYSA-N [butyl(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(CCCC)OC1=CC=CC=C1 LKMDHQMGVTVIRI-UHFFFAOYSA-N 0.000 claims description 2
- KDXRHNQIWBGFLG-UHFFFAOYSA-N [hexyl(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(CCCCCC)OC1=CC=CC=C1 KDXRHNQIWBGFLG-UHFFFAOYSA-N 0.000 claims description 2
- GRKDCROEGSBEOZ-UHFFFAOYSA-N [pentyl(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(CCCCC)OC1=CC=CC=C1 GRKDCROEGSBEOZ-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims 8
- 239000000463 material Substances 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 12
- 229910017604 nitric acid Inorganic materials 0.000 description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 229910052761 rare earth metal Inorganic materials 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 238000011068 loading method Methods 0.000 description 6
- 239000002893 slag Substances 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- 229910052590 monazite Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000007818 Grignard reagent Substances 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- BHIIGRBMZRSDRI-UHFFFAOYSA-N [chloro(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(Cl)OC1=CC=CC=C1 BHIIGRBMZRSDRI-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- HAKMAMKAFTZXOZ-UHFFFAOYSA-N dioctoxyphosphorylbenzene Chemical compound CCCCCCCCOP(=O)(OCCCCCCCC)C1=CC=CC=C1 HAKMAMKAFTZXOZ-UHFFFAOYSA-N 0.000 description 2
- 239000012527 feed solution Substances 0.000 description 2
- 230000004992 fission Effects 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000001347 alkyl bromides Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- DMSZORWOGDLWGN-UHFFFAOYSA-N ctk1a3526 Chemical compound NP(N)(N)=O DMSZORWOGDLWGN-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 150000004795 grignard reagents Chemical class 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/387—Cyclic or polycyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/30—Phosphinic acids [R2P(=O)(OH)]; Thiophosphinic acids ; [R2P(=X1)(X2H) (X1, X2 are each independently O, S or Se)]
- C07F9/32—Esters thereof
- C07F9/3205—Esters thereof the acid moiety containing a substituent or a structure which is considered as characteristic
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/30—Phosphinic acids [R2P(=O)(OH)]; Thiophosphinic acids ; [R2P(=X1)(X2H) (X1, X2 are each independently O, S or Se)]
- C07F9/32—Esters thereof
- C07F9/3258—Esters thereof the ester moiety containing a substituent or a structure which is considered as characteristic
- C07F9/3282—Esters with hydroxyaryl compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/40—Esters thereof
- C07F9/4003—Esters thereof the acid moiety containing a substituent or a structure which is considered as characteristic
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/40—Esters thereof
- C07F9/4071—Esters thereof the ester moiety containing a substituent or a structure which is considered as characteristic
- C07F9/4084—Esters with hydroxyaryl compounds
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- General Health & Medical Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Geology (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Extraction Or Liquid Replacement (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a kind of extraction separating method of thorium, the method is used as extractant using at least one of neutrality phosphine extractant shown in logical formula (I), the thorium in extraction and separation thoriated material liquid；Wherein R1Selected from C1~C8Alkyl and H, R2Selected from C1~C8Alkyl and H, R3Selected from C1~C8Linear or branched alkyl group, R4Selected from phenoxy group or C1~C8Linear or branched alkyl group.Extractant of the invention and the extraction system that diluent forms are high to the extraction yield of the thorium in thoriated material liquid, and have very high load capacity to thorium, are a kind of extraction separating methods of efficient thorium.
Description
Technical Field
The invention relates to the field of extraction and separation of thorium, in particular to a method for extracting and separating thorium by using a novel neutral phosphine extracting agent.
Background
Thorium is an important potential nuclear energy fuel, is not easy to fission, but can be converted into U-233 which is easy to fission after absorbing neutrons, and can be used as a raw material of a novel nuclear reactor for power generation, so that the purification and preparation of thorium are important preconditions for thorium nuclear energy development. At present, in Jiangxi province and other regions in the south of China, ion adsorption type rare earth ores are accompanied by low-radioactivity thorium, the utilization rate of the thorium is almost zero, and the thorium enters slag and tailings along with the exploitation of rare earth and is used as a non-recovered byproduct, so that the environment is greatly polluted and damaged.
The method for extracting thorium from nitric acid solution by tributyl phosphate (TBP) is most widely applied at the earliest time. TBP has stable property, is not oxidized by nitric acid, and has low price. However, the extractant needs to be pretreated to remove some impurities in the TBP before use, and needs to be washed with dilute nitric acid, so that a large amount of acid is consumed. Furthermore, TBP is also hydrolyzed to some extent during the extraction process, which results in the consumption of large amounts of extractant. Chinese patent CN104131164A discloses a method for extracting and separating thorium by using a neutral phosphoramide extractant, which can realize effective separation of thorium by using a short extraction flow, but the method also has the problems of large dosage of the extractant, relatively low thorium-loaded capacity (the loaded amount of 30% of the extractant to thorium is 48.56g/L) and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for extracting and separating thorium by using the neutral phosphine extracting agent, the extracting agent has high separation coefficient and good extraction phenomenon, and the extracting agent has good stability and high repeated utilization rate, and is obviously improved.
Therefore, the invention provides the following technical scheme:
the invention provides a method for extracting and separating thorium, which adopts at least one of neutral phosphine extracting agents shown in a general formula (I) as an extracting agent to extract and separate thorium in a thorium-containing raw material liquid:
wherein,
R1is selected from C1～C8Alkyl and H, preferably from C1～C4Alkyl and H, more preferably from C1～C2Alkyl and H;
R2is selected from C1～C8Alkyl and H, preferably from C1～C4Alkyl and H, more preferably from C1～C2Alkyl and H;
R3is selected from C1～C8Straight-chain or branched alkyl, preferably from C3～C7Straight or branched alkyl, more preferably from C3～C7A linear alkyl group.
R4Selected from phenoxy or C1～C8Straight or branched alkyl, preferably from phenoxy or C4～C8Straight or branched chain alkyl, more preferably from phenoxy.
Preferably, in the neutral phosphine extractant of the formula (I), R1、R2And R3The total carbon number of (a) is 1 to 28, preferably 2 to 16, more preferably 3 to 10, and still more preferably 4 to 8.
Preferably, in the neutral phosphine extractant of the formula (I), R1、R2、R3And R4The total carbon number of (a) is 1 to 36, preferably 8 to 22, more preferably 9 to 16, and still more preferably 10 to 14.
Preferred neutral phosphine extractants of the formula (I) are one or more of diphenyl n-butylphosphonate, diphenyl isobutylphosphonate, diphenyl tert-butylphosphonate, diphenyl n-pentylphosphonate, diphenyl isopentylphosphonate, diphenyl n-hexylphosphonate, diphenyl isohexylphosphonate, diphenyl n-heptylphosphonate, diphenyl isoheptylphosphonate, diphenyl n-octylphosphonate, diphenyl isooctylphosphonate, phenyl di-n-butylphosphonate, phenyl di-tert-butylphosphonate, phenyl diisohexylphosphonate, phenyl di-n-hexylphosphonate and phenyl di-n-octylphosphonate in any desired proportions. Also preferred is a neutral phosphine extractant of the formula (I) which is a mixture of one or more of tert-butyl diphenyl phosphonate, n-octyl diphenyl phosphonate, di-tert-butyl phenyl phosphonate and di-n-octyl phenyl phosphonate in any proportion.
According to the invention, the method comprises the following steps: mixing at least one neutral phosphine extracting agent shown in the general formula (I) with a diluent to form an organic phase, mixing the organic phase with a thorium-containing raw material liquid, and extracting, so that thorium is separated from the raw material liquid and enters the organic phase to obtain a thorium-containing extract liquid.
According to the invention, the method further comprises the following steps: and (3) back-extracting the thorium-containing extract by using a back-extracting agent (also called back-extracting solution, back-extracting solution or back-extracting solution) to obtain a back-extracted product containing thorium.
According to the invention, the process further comprises, before the stripping step, a washing step, i.e. a step of washing the thorium-containing extract with a washing liquid (which may also be referred to as washing liquid, washing acid, washing agent).
According to the invention, the extraction temperature is preferably 20-40 ℃, more preferably 25-30 ℃, and the extraction time is preferably 5-30 min, more preferably 10-20 min. The back extraction temperature is preferably 20-40 ℃, more preferably 25-30 ℃, and the back extraction time is preferably 5-30 min, more preferably 10-20 min.
The invention has the beneficial effects that:
compared with the prior art, the invention provides a thorium extraction and separation method, wherein a brand-new extracting agent (one or more of neutral phosphine extracting agents shown in a formula (I)) is adopted, the extracting capability of the extracting agent is strong, and particularly, the extraction rate of a thorium solution (thorium-containing raw material liquid) with higher concentration can reach more than 90%; in addition, the extraction agent has low dosage and high loading capacity (the loading capacity of the extraction agent with the volume fraction of about 0.5 percent to thorium reaches 130mg/L), and the extraction agent has no extraction capacity to rare earth elements, can achieve the best separation effect in the shortest time, realizes effective separation and recovery of thorium, and has high application value.
Drawings
FIG. 1 extraction yield of different extractants according to the invention
FIG. 2 thorium loading of different extractants of the invention and of the prior art (concentration 0.015mol/L, volume fraction about 0.5%)
Detailed Description
As mentioned above, the invention provides a method for extracting and separating thorium, wherein at least one neutral phosphine extraction agent shown as a general formula (I) is used for extracting and separating thorium in a thorium-containing raw material liquid:
wherein
R1Is selected from C1～C8Alkyl and H, preferably from C1～C4Alkyl and H, more preferably from C1～C2Alkyl and H;
R2is selected from C1～C8Alkyl and H, preferably from C1～C4Alkyl and H, more preferably from C1～C2Alkyl and H;
R3is selected from C1～C8Straight-chain or branched alkyl, preferably from C3～C7Straight or branched alkyl, more preferably from C3～C7A linear alkyl group.
R4Is selected from phenoxy or C1-C8 straight chain or branched chain alkyl, preferably from phenoxy or C4-C8 straight chain or branched chain alkyl, more preferably from phenoxy.
Preferably, in the neutral phosphine extractant of the formula (I), R1、R2And R3The total carbon number of (a) is 1 to 28, preferably 2 to 16, more preferably 3 to 10, and still more preferably 4 to 8.
Preferably, in the neutral phosphine extractant of the formula (I), R1、R2、R3And R4The total carbon number of (a) is 1 to 36, preferably 8 to 22, more preferably 9 to 16, and still more preferably 10 to 14.
In a preferred embodiment of the invention, the method comprises the steps of: mixing at least one neutral phosphine extracting agent shown in the general formula (I) with a diluent to form an organic phase, mixing the organic phase with a thorium-containing raw material liquid, and extracting, so that thorium is separated from the raw material liquid and enters the organic phase to obtain a thorium-containing extract liquid.
It has been found that after the extraction of the organic phase containing the neutral phosphine extractant mixed with the thorium-containing feed solution, the neutral phosphine extractant forms a thorium-containing organic complex with thorium, thereby separating thorium from the feed solution into the organic phase and obtaining a thorium-containing extract.
The diluent comprises one or more of an alkane or an arene. Preferably, the alkane is selected from one or more of n-heptane, octane, hexadecane, aviation kerosene or No. 260 solvent naphtha; the aromatic hydrocarbon is selected from one or more of benzene, toluene and xylene. More preferably, the diluent is selected from one or more of benzene, toluene and xylene.
The volume ratio of the neutral phosphine extraction agent to the diluent is 1-50: 50-99, preferably 10-40: 60-90, more preferably 10-30: 70-90. Research finds that the extraction phenomenon can be improved by properly adding the diluent, and when the diluent is excessive, the proportion of the extracting agent in an extraction system is reduced, so that the extraction capacity is influenced; when the amount of the diluent is too small, the viscosity of the organic phase in the extraction system and thus the extraction phenomenon are affected, so that an appropriate volume ratio is selected.
The thorium-containing raw material liquid contains thorium, inorganic acid and other non-thorium elements. The non-thorium element can be a rare earth element, an alkali metal element, an alkaline earth metal element, a transition metal element or a non-metal element and the like; preferably, the non-thorium element is a rare earth element. The concentration of thorium in the thorium-containing raw material liquid is not particularly limited, and may be preferably 0.00001mol/L to 0.001mol/L, more preferably 0.00001mol/L to 0.0005mol/L, and still more preferably 0.00005mol/L to 0.0005 mol/L. Preferably, the inorganic acid in the raw material liquid is selected from hydrochloric acid, sulfuric acid or nitric acid, preferably hydrochloric acid or nitric acid, and more preferably nitric acid. The acidity (hydrogen ion concentration) of the raw material liquid is preferably 0.01 to 6mol/L, and more preferably 0.1 to 3 mol/L. Too high or too low acidity of the feed liquid affects the extraction yield or the extraction phenomenon. The concentration of the non-thorium element is not particularly limited, and may preferably be 0.01 to 0.1 mol/L. The starting material of the thorium-containing starting material liquid is not particularly limited as long as thorium is contained therein. For example, thoriated ores, thoriated slags or thorium concentrates, etc. may be selected; the thorium-containing ore is, for example, monazite ore, bastnaesite ore or a mixed ore of the monazite ore and the bastnaesite ore; the thorium-containing slag is, for example, monazite slag, bastnaesite slag, or a mixed slag of the two, or the like. The above-mentioned raw materials are pretreated and dissolved in inorganic acid so as to obtain the thorium-containing raw material liquor suitable for said invention.
In a preferred embodiment of the present invention, the method further comprises the steps of: and (3) back-extracting the thorium-containing extract by using a back-extracting agent (also called back-extracting solution, back-extracting solution or back-extracting solution) to obtain a back-extracted product containing thorium. The stripping solution can be nitric acid, hydrochloric acid, sulfuric acid or a mixed solution of the above acids, or an aqueous solution of carbonate, and the carbonate can be an alkali metal salt, an alkaline earth metal salt or an ammonium salt, such as a sodium salt, a potassium salt and the like. Preferably, when the acid solution is used as the stripping solution, the acidity is about 0.05-2 mol/L calculated by the molar concentration of hydrogen ions; when a carbonate aqueous solution is used as the stripping solution, the concentration thereof may be about 0.5 to 5 wt%. Preferably, the stripping solution is dilute nitric acid with the concentration of about 0.1-0.5 mol/L or sodium carbonate aqueous solution with the concentration of about 0.5-3 wt%.
In a preferred embodiment of the invention, the process further comprises, before the stripping step, a washing step, i.e. a step of washing the thorium-containing extract with a washing liquid (which may also be referred to as wash liquid, wash acid, detergent). The washing solution can be nitric acid, sulfuric acid, hydrochloric acid or a mixed solution of the above acids in any proportion. The acidity of the washing solution may be about 0.2 to 0.8mol/L, calculated as the molar concentration of hydrogen ions.
The extraction temperature is preferably 20-40 ℃, more preferably 25-30 ℃, and the extraction time is preferably 5-30 min, more preferably 10-20 min. The back extraction temperature is preferably 20-40 ℃, more preferably 25-30 ℃, and the back extraction time is preferably 5-30 min, more preferably 10-20 min.
After the extraction separation is finished, the content of thorium element in the raffinate or the strip liquor obtained by the method is preferably determined by an ICP-OES method.
The extraction rate and the back extraction rate which are required to be obtained are calculated by the following formulas:
wherein [ M]tOriginal concentration of thorium, [ M ]]aIs the equilibrium concentration of thorium, [ M ]]aq,aFor the thorium concentration at the reextraction equilibrium, [ M ]]org,tIs the thorium concentration in the organic phase after extraction.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the description of the present invention, and such equivalents also fall within the scope of the invention.
Reagents and sources
Hydrochloric acid (analytically pure); sulfuric acid (analytically pure); nitric acid (analytically pure); sodium nitrate (analytical grade); anhydrous ether (analytical grade); toluene (analytically pure) was purchased from the national pharmaceutical group chemical reagents, Inc. Diphenyl chlorophosphate (CAS: 2524-63-3), magnesium chloride, and alkyl bromide were all available from Seasa reagent.
The NMR instrument is AV III-500 BRUKER.
The product purity was determined by ICP-OES (Horiba Ultima 2).
Preparation example 1
Anhydrous ether is used as a solvent, and a stirrer, a constant pressure funnel and a reflux condensing device with nitrogen protection are arranged on a 250mL three-neck flask. Adding into a flaskAdding the halohydrocarbon R into the anhydrous ether solution and the magnesium strip under stirring1R2R3CX (wherein, R)1、R2And R3As defined above, X is selected from halogen), a grignard reagent in ether solution is prepared.
Using anhydrous ether as solvent, adding diphenyl chlorophosphate (or chloroalkylphenyl phosphonate, the alkyl is C1～C8Straight or branched alkyl, preferably C4～C8Straight chain or branched chain alkyl) and the prepared Grignard reagent diethyl ether solution, reacting overnight, layering, drying diethyl ether layer, suction filtering, and distilling residue under reduced pressure to obtain the final product of crude product purification.
When R is1＝R2＝R3Methyl, R4When phenoxy, the extractant of formula a below (diphenyl tert-butylphosphonate) is obtained; when R is1＝R2＝H、R3＝n-C7H15、R4When phenoxy, an extractant of formula B below (diphenyl n-octylphosphonate, noted ODP) is obtained; when R is1＝R2＝R3Methyl, R4When the compound is tert-butyl, an extractant of the following formula C (di-tert-butyl phenyl phosphonate) is obtained; when R is1＝R2＝H、R3＝n-C7H15、R4When n-octyl, the extractant of formula D below (di-n-octylphenyl phosphonate) is obtained.
Example 1
The organic phase was configured: one of the extractants synthesized in preparation example 1 was mixed with toluene to form an organic phase, and the concentration of the extractant was 0.035 mol/L.
Preparing a thorium-containing raw material liquid: respectively taking thorium and a single solution of rare earth lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium, adding dilute nitric acid to prepare a thorium-containing raw material liquid with the total rare earth concentration of 0.01mol/L, the single rare earth concentration of 0.00067mol/L and the thorium concentration of 0.001mol/L, wherein the acidity (hydrogen ion concentration) of the thorium-containing raw material liquid is 1 mol/L.
And mixing the organic phase and the thorium-containing raw material liquid according to the volume ratio of 1:1, extracting at room temperature, and calculating the extraction rate E% after the extraction is finished.
Table 1 extraction of thorium from example 1
| The extraction rate E% | |
| An extractant shown as formula A | 99.7 |
| An extractant shown as a formula B | 94.1 |
The results of the extraction with the extractants of formula a and formula B above, respectively, are shown in figure 1. As can be seen from fig. 1, the extractant shown in formula a has the best separation effect on thorium, but the extractant shown in formula B also has the best separation effect on thorium and has higher selectivity on thorium.
Example 2
The organic phase was configured: the extractant of formula B synthesized in preparation example 1 was mixed with toluene to form an organic phase, the concentration of the extractant was 0.015mol/L and the volume fraction was about 0.5%.
Preparing a thorium-containing raw material liquid: taking a single thorium solution, adding dilute nitric acid to prepare a thorium-containing raw material liquid with thorium concentration of 0.0005mol/L, wherein the acidity (hydrogen ion concentration) of the thorium-containing raw material liquid is 1 mol/L.
Mixing the organic phase and the thorium-containing raw material liquid according to the volume ratio of 1:1, extracting for multiple times at room temperature, and calculating the loading capacity after the extraction is finished.
The extractant of formula B (about 0.5% by volume) was found to achieve a loading of 130mg/L of thorium (see FIG. 2 and Table 2).
TABLE 2
As can be seen from Table 2, the loading of thorium by the extractant (volume fraction about 0.5%) of the invention is as high as 130.7mg/L compared with the existing extractant, which is much higher than that of the existing extractant.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (28)
1. The method for extracting and separating thorium is characterized in that at least one of neutral phosphine extracting agents shown in a general formula (I) is used as an extracting agent to extract and separate thorium in a thorium-containing raw material liquid:
wherein,
R1is selected from C1～C8Alkyl and H;
R2is selected from C1～C8Alkyl and H;
R3is selected from C1～C8A linear or branched alkyl group;
R4is selected from phenoxy or C1-C8 straight chain or branched chain alkyl.
2. Process for the extractive separation of thorium according to claim 1, in which R1Is selected from C1～C4Alkyl and H.
3. Process for the extractive separation of thorium according to claim 2, in which R1Is selected from C1～C2Alkyl and H.
4. Process for the extractive separation of thorium according to claim 1, in which R2Is selected from C1～C4Alkyl and H.
5. Process for the extractive separation of thorium according to claim 4, in which R2Is selected from C1～C2Alkyl and H.
6. Process for the extractive separation of thorium according to claim 1, in which R3Is selected from C3～C7Straight or branched chain alkyl.
7. Process for the extractive separation of thorium according to claim 6, in which R3Is selected from C3～C7A linear alkyl group.
8. Process for the extractive separation of thorium according to claim 1, in which R4Is selected from phenoxy or C4-C8 straight chain or branched chain alkyl.
9. Process for the extractive separation of thorium according to claim 8, which consists inIn, R4Is selected from phenoxy.
10. The process for the extractive separation of thorium according to claim 1, characterized in that in the neutral phosphine extractant of the general formula (I), R is1、R2And R3The total number of carbon atoms of (1) to (28).
11. The process for the extractive separation of thorium according to claim 10, characterized in that in the neutral phosphine extractant of the general formula (I), R is1、R2And R3The total number of carbon atoms of (2) to (16).
12. The process for the extractive separation of thorium according to claim 11, characterized in that in the neutral phosphine extractant of the general formula (I), R is1、R2And R3The total number of carbon atoms of (2) is 3 to 10.
13. The process for the extractive separation of thorium according to claim 12, characterized in that in the neutral phosphine extractant of the general formula (I), R is1、R2And R3The total number of carbon atoms of (2) is 4 to 8.
14. The process for the extractive separation of thorium according to claim 10, characterized in that in the neutral phosphine extractant of the general formula (I), R is1、R2、R3And R4The total number of carbon atoms of (1) to (36).
15. The process for the extractive separation of thorium according to claim 14, characterized in that in the neutral phosphine extractant of the general formula (I), R is1、R2、R3And R4The total number of carbon atoms of (2) is 8 to 22.
16. Process for the extractive separation of thorium according to claim 15, characterized in that it consists in a process for the extractive separation of thorium of general formula(I) In the neutral phosphine extractant shown, R1、R2、R3And R4The total number of carbon atoms of (A) is 9 to 16.
17. The process for the extractive separation of thorium according to claim 16, characterized in that in the neutral phosphine extractant of the general formula (I), R is1、R2、R3And R4The total number of carbon atoms of (A) is 10 to 14.
18. The process for the extractive separation of thorium according to claim 1, wherein the neutral phosphine extractant represented by the general formula (I) is one or a mixture of more of diphenyl n-butylphosphonate, diphenyl isobutylphosphonate, diphenyl tert-butylphosphonate, diphenyl n-pentylphosphonate, diphenyl isopentylphosphonate, diphenyl n-hexylphosphonate, diphenyl isohexylphosphonate, diphenyl n-heptylphosphonate, diphenyl isoheptylphosphonate, diphenyl n-octylphosphonate, diphenyl isooctylphosphonate, phenyl di-n-butylphosphonate, phenyl diisobutylphosphonate, phenyl di-tert-butylphosphonate, phenyl diisohexylphosphonate, phenyl di-n-hexylphosphonate and phenyl di-n-octylphosphonate in any proportion.
19. The process for the extractive separation of thorium according to claim 18, wherein the neutral phosphine extractant represented by the general formula (I) is a mixture of one or more of diphenyl tert-butylphosphonate, diphenyl n-octylphosphonate, phenyl di-tert-butylphosphonate and phenyl di-n-octylphosphonate in any proportion.
20. A process for the extractive separation of thorium according to any of claims 1 to 19, characterized in that it comprises the following steps: mixing at least one neutral phosphine extracting agent shown in the general formula (I) with a diluent to form an organic phase, mixing the organic phase with a thorium-containing raw material liquid, and extracting, so that thorium is separated from the raw material liquid and enters the organic phase to obtain a thorium-containing extract liquid.
21. Process for the extractive separation of thorium according to claim 20, characterized in that it also comprises the further steps of: and (3) back-extracting the thorium-containing extract liquor by using a back-extracting agent to obtain a back-extracted product containing thorium.
22. Process for the extractive separation of thorium according to claim 21, characterized in that it comprises, before the back-extraction step, a washing step, i.e. a washing step of the thorium-containing extract with a washing liquid.
23. The extraction separation method of thorium according to claim 20, characterized in that the temperature of the extraction is 20 to 40 ℃ and the time of the extraction is 5 to 30 min.
24. The method for the extractive separation of thorium according to claim 23, characterized in that the temperature of the extraction is 25 to 30 ℃.
25. The method for the extractive separation of thorium according to claim 24, wherein the time for the extraction is 10 to 20 min.
26. The extraction separation method of thorium according to claim 21, wherein the back extraction temperature is 20-40 ℃ and the back extraction time is 5-30 min.
27. The method for the extractive separation of thorium according to claim 26, wherein the temperature of the back extraction is 25-30 ℃.
28. The extraction separation method of thorium according to claim 27, wherein the back extraction time is 10-20 min.
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