NO885728L - ION EXCHANGE METHOD FOR SEPARATING SCANDIUM AND THORIUM. - Google Patents
ION EXCHANGE METHOD FOR SEPARATING SCANDIUM AND THORIUM.Info
- Publication number
- NO885728L NO885728L NO885728A NO885728A NO885728L NO 885728 L NO885728 L NO 885728L NO 885728 A NO885728 A NO 885728A NO 885728 A NO885728 A NO 885728A NO 885728 L NO885728 L NO 885728L
- Authority
- NO
- Norway
- Prior art keywords
- thorium
- scandium
- solution
- elution
- separating
- Prior art date
Links
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 title claims description 34
- 229910052776 Thorium Inorganic materials 0.000 title claims description 34
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 title claims description 34
- 229910052706 scandium Inorganic materials 0.000 title claims description 33
- 238000000034 method Methods 0.000 title claims description 14
- 238000005342 ion exchange Methods 0.000 title description 3
- 239000000243 solution Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000010828 elution Methods 0.000 claims description 13
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003729 cation exchange resin Substances 0.000 claims description 9
- QEVGZEDELICMKH-UHFFFAOYSA-N Diglycolic acid Chemical compound OC(=O)COCC(O)=O QEVGZEDELICMKH-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 claims 1
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- TXBBUSUXYMIVOS-UHFFFAOYSA-N thenoyltrifluoroacetone Chemical compound FC(F)(F)C(=O)CC(=O)C1=CC=CS1 TXBBUSUXYMIVOS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000658 coextraction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000000248 direct current plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical group [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000012607 strong cation exchange resin Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
Oppfinnelsens områdeField of the invention
Denne oppfinnelse angår en metode for separering av skandium og thorium. Denne oppfinnelse angår mer spesielt en ionebyttemetode for separering av scandium og thorium. This invention relates to a method for separating scandium and thorium. This invention relates more particularly to an ion exchange method for separating scandium and thorium.
Oppfinnelsens bakgrunnThe background of the invention
Skandium og thorium er to metaller som erkarakterisertved et høyt forhold mellom ladning og radius. De er derfor tilbøyelige til å oppføre seg på lignende måte ved de kom-pleksdannende reaksjoner som er grunnlaget for hydrometal-lurgiske separasjoner. Når for eksempel skandium ekstra-heres fra oppløsningen av wolframoppslutningsslam med thenoyltrifluoraceton (TTA), er thorium det eneste element som blir samekstrahert i betydelige mengder selv om flere enn ett dusin andre elementer er tilstede i oppløsningen. Den kvantitative separering av skandium fra thorium ved en enkel utfelling eller ekstraksjon er dessuten ekstremt vanskelig på grunn av denne likhet i de kjemiske egenskaper til ionene i oppløsning og som forårsaker samekstraksjon. Dette problem kan tas hånd om på en tilfredsstillende måte ved hjelp av den her beskrevne prosess. Scandium and thorium are two metals that are characterized by a high ratio between charge and radius. They are therefore inclined to behave in a similar way in the complex-forming reactions which are the basis for hydrometallurgical separations. For example, when scandium is extracted from the solution of tungsten digestion sludge with thenoyltrifluoroacetone (TTA), thorium is the only element that is co-extracted in significant amounts even though more than a dozen other elements are present in the solution. The quantitative separation of scandium from thorium by a simple precipitation or extraction is moreover extremely difficult because of this similarity in the chemical properties of the ions in solution which causes co-extraction. This problem can be dealt with satisfactorily using the process described here.
Oppsummering av oppfinnelsenSummary of the invention
I overensstemmelsen med én side av den foreliggende oppfinnelse omfatter en ny og forbedret metode for separer-ingen av skandium og thorium de følgende trinn: Trinn 1 - En oppløsning som omfatter skandium og thorium innstilles på en sur pH for å In accordance with one aspect of the present invention, a new and improved method for the separation of scandium and thorium comprises the following steps: Step 1 - A solution comprising scandium and thorium is adjusted to an acidic pH to
danne en sur oppløsning.form an acidic solution.
Trinn 2 - Syreoppløsningen fra trinn 1 kontaktes med Step 2 - The acid solution from step 1 is contacted with
en kationbytteharpiks.a cation exchange resin.
Trinn 3 - Skandiumet og thoriumet beholdes på kationbytteharpiks en . Step 3 - The scandium and thorium are retained on a cation exchange resin.
Trinn 4 - Skandiumet fra kationbytteharpiksen Step 4 - The scandium from the cation exchange resin
elueres med en første elueringsoppløsning. eluted with a first elution solution.
Trin 5 - Thoriumet fra kationbytteharpiksen elueres med en annen elueringsoppløsning. Step 5 - The thorium from the cation exchange resin is eluted with another elution solution.
Kortfattet beskrivelse av tegningenBrief description of the drawing
På tegningen:On the drawing:
Den eneste figur er en kurve over konsentrasjonen av skandium og thorium som en funksjon av fraksjonsnummeret for avløpsstrømmen i overensstemmelse med den foreliggende oppfinnelse . The only figure is a curve of the concentration of scandium and thorium as a function of the fraction number of the effluent stream in accordance with the present invention.
For en bedre forståelse av den foreliggende oppfinnelse sammen med andre og ytterligere formål, fordeler og muligheter ved denne gjøres henvisning til den følgende beskrivelse og de vedføyede krav i forbindelse med den oven-for beskrevne tegning. For a better understanding of the present invention together with other and further purposes, advantages and possibilities thereof, reference is made to the following description and the appended claims in connection with the above-described drawing.
Detaljert beskrivelse av oppfinnelsenDetailed description of the invention
Ved fremgangsmåten ifølge den foreliggende oppfinnelse er metallene skandium og thorium som er tilstede i selv meget fortynnede oppløsninger, blitt fullstendig adsorbert av en sterk kationbytteharpiks i hydrogenformen. Efter at harpiksen er blitt belastet med metallene, ble skandium eluert selektivt efterlatende thoriumet på harpiksen. Thoriumet ble senere eluert under andre betingelser. På denne måte ble begge metaller konsentrert, i adsorpsjonstrinnet, og fullstendig separert fra hverandre i elueringstrinnet(ene). In the method according to the present invention, the metals scandium and thorium, which are present even in very dilute solutions, have been completely adsorbed by a strong cation exchange resin in the hydrogen form. After the resin was loaded with the metals, the scandium was eluted selectively leaving the thorium on the resin. The thorium was later eluted under other conditions. In this way, both metals were concentrated, in the adsorption step, and completely separated from each other in the elution step(s).
EksempelExample
Én liter av en oppløsning inneholdende 25 ppm skandium og 25 ppm thorium ble innstilt på en pH av 1,95. En ionebyttekolonne bestående av 10 g av en kationbytteharpiks med en sulfonsyrefunksjonalitet, som Amberlite 1R-118(+) One liter of a solution containing 25 ppm scandium and 25 ppm thorium was adjusted to a pH of 1.95. An ion exchange column consisting of 10 g of a cation exchange resin with a sulfonic acid functionality, such as Amberlite 1R-118(+)
(Rohm og Haas ionebytteharpiks), ble fremstilt og omvandlet til hydrogenioneformen ved å lede 1 N saltsyre gjennom kolonnen inntil avløpsstrømmen var sur. Deionisert vann ble derefter presset gjennom kolonnen inntil avløpsstrømmen var nøytral. Det oppnådde harpikslag hadde et tverrsnitts-areal pa ca. 1 cm 2 og en lengde pa 10 cm. Oppløsningen av skandium og thorium ble derefter ledet gjennom denne kolonne med en strømningshastighet på 4 ml pr. minutt. Avløpsstrømmen ble oppsamlet som en enkelt 1 liters fraksjon, og skandium- og thoriumkonsentrasjonene i denne avløps- (Rohm and Haas ion exchange resin), was prepared and converted to the hydrogen ion form by passing 1 N hydrochloric acid through the column until the effluent stream was acidic. Deionized water was then forced through the column until the effluent stream was neutral. The resulting resin layer had a cross-sectional area of approx. 1 cm 2 and a length of 10 cm. The solution of scandium and thorium was then passed through this column at a flow rate of 4 ml per minute. minute. The effluent stream was collected as a single 1 liter fraction, and the scandium and thorium concentrations in this effluent
strøm ble funnet å være langt lavere enn 0,05 ppm. Da kon-sentrasjonene i mateoppløsningen var 25 ppm, var adsorp-sjonen av begge metaller på harpiksen lik eller større enn 99,8%. current was found to be far lower than 0.05 ppm. When the concentrations in the feed solution were 25 ppm, the adsorption of both metals on the resin was equal to or greater than 99.8%.
Eluering av skandium fra harpiksen ble oppnådd med et elueringsmiddel bestående av en oppløsning av diglycolsyre i saltsyre. Konsentrasjonen av diglycolsyre var 0,1 M, og konsentrasjonen av saltsyre var 1,2 M. Da eluering av skandium var nesten fullstendig, ble eluerings-midlet skiftet til ren 6N saltsyre for å fortrenge thorium fra harpiksen. Avløpsstrømmen ble oppsamlet i like volum-fraksjoner på 5 milliliter for analytiske formål. Skandium-og thoriumkonsentrasjoner i disse fraksjoner ble bestemt ved Likestrømsplasmaatomemisjonsspektroskopi (DCP). Resultatene er gjengitt i Tabell 1 og vist på den eneste figur. Det er klart ut fra resultatene at i det vesentlige en fullstendig separering av skandium og thorium er blitt oppnådd. Elution of scandium from the resin was achieved with an eluent consisting of a solution of diglycolic acid in hydrochloric acid. The concentration of diglycolic acid was 0.1 M, and the concentration of hydrochloric acid was 1.2 M. When elution of scandium was almost complete, the eluent was changed to pure 6N hydrochloric acid to displace thorium from the resin. The effluent stream was collected in equal volume fractions of 5 milliliters for analytical purposes. Scandium and thorium concentrations in these fractions were determined by direct current plasma atomic emission spectroscopy (DCP). The results are reproduced in Table 1 and shown in the only figure. It is clear from the results that essentially a complete separation of scandium and thorium has been achieved.
På grunn av den lille overlapping mellom skandium- Because of the small overlap between scandium-
og thoriumtoppene vil den gjenvundne prosent skandium og renheten bli innbyrdes forbundet. Det vil si at velging av 100% skandiumgjenvinning vil føre til noen grad av for-urensning med thorium. Forurensningsomfanget som funksjon av utvinningen kan beregnes ved å integrere elueringskurvene. Disse beregninger er blitt utført for fraksjonene innen over-lappingsområdet. Resultatene er vist i Tabell 2. and the thorium peaks, the recovered percent scandium and the purity will be interconnected. This means that choosing 100% scandium recovery will lead to some degree of contamination with thorium. The extent of contamination as a function of recovery can be calculated by integrating the elution curves. These calculations have been carried out for the fractions within the overlapping area. The results are shown in Table 2.
Disse resultater antyder at dersom fraksjon 28 tas som en avskjæring, vil 95-96% av skandiumet være blitt eluert forurenset med bare ca. 0,1% thorium. På den annen side når fraksjon 32 tas som en avskjæring for å øke skandiumgjenvinning til 99,5%, vil et produkt forurenset med 1,1% thorium fås. These results suggest that if fraction 28 is taken as a cutoff, 95-96% of the scandium will have been eluted contaminated with only approx. 0.1% thorium. On the other hand, when fraction 32 is taken as a cutoff to increase scandium recovery to 99.5%, a product contaminated with 1.1% thorium will be obtained.
Fordelen med den foreliggende fremgangsmåte sammen-lignet med tidligere metoder er evnen til å arbeide ved omgivelsestemperatur under utelukkelse av mer kostbar be-arbeiding . The advantage of the present method compared to previous methods is the ability to work at ambient temperature while excluding more expensive processing.
Selv om det som for tiden betraktes som de foretrukne utførelsesformer av oppfinnelsen er blitt beskrevet, vil det være selvklart for fagfolk at forskjellige forandringer av denne kan foretas uten å avvike fra oppfinnelsens omfang som definert ved de vedføyede krav. Although what are currently considered to be the preferred embodiments of the invention have been described, it will be self-evident to those skilled in the art that various changes thereof can be made without deviating from the scope of the invention as defined by the appended claims.
Claims (6)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US07/042,150 US4765909A (en) | 1987-04-23 | 1987-04-23 | Ion exchange method for separation of scandium and thorium |
PCT/US1988/001207 WO1988008323A1 (en) | 1987-04-23 | 1988-04-12 | Ion exchange method for separation of scandium and thorium |
Publications (2)
Publication Number | Publication Date |
---|---|
NO885728L true NO885728L (en) | 1988-12-22 |
NO885728D0 NO885728D0 (en) | 1988-12-22 |
Family
ID=26718925
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
NO885728A NO885728D0 (en) | 1987-04-23 | 1988-12-22 | ION EXCHANGE METHOD FOR SEPARATING SCANDIUM AND THORIUM. |
Country Status (1)
Country | Link |
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NO (1) | NO885728D0 (en) |
-
1988
- 1988-12-22 NO NO885728A patent/NO885728D0/en unknown
Also Published As
Publication number | Publication date |
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NO885728D0 (en) | 1988-12-22 |
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