CS238421B1 - Cation resin preparation method with dithiocarbamate group - Google Patents

Cation resin preparation method with dithiocarbamate group Download PDF

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CS238421B1
CS238421B1 CS559783A CS559783A CS238421B1 CS 238421 B1 CS238421 B1 CS 238421B1 CS 559783 A CS559783 A CS 559783A CS 559783 A CS559783 A CS 559783A CS 238421 B1 CS238421 B1 CS 238421B1
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Czechoslovakia
Prior art keywords
anion
dithiocarbamate group
exchange resin
dithiocarbamate
group
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CS559783A
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Czech (cs)
Slovak (sk)
Inventor
Zdenek Hladky
Vladimir Rattay
Juliana Risova
Jozef Polonsky
Jan Gargaj
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Zdenek Hladky
Vladimir Rattay
Juliana Risova
Jozef Polonsky
Jan Gargaj
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Priority to CS559783A priority Critical patent/CS238421B1/en
Publication of CS238421B1 publication Critical patent/CS238421B1/en

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Abstract

Vynález rieši sposob přípravy katexu s ditiokarbamátovou skupinou. Postupuje sa tak, že anex obsahujúci najma sekundárné aminové skupiny v aktivně) formě sa nechá 24 hodin vo vodnom roztoku hydrooxidu amonného alebo hydroxidu alkalického upraveného na hodnotu pH 7,5 až 9 napuČať. Po odfiltrovaní sa anex premyje destilovanou vodou a na 1 milimól výmennej kapacity anexu sa přidává 1 milimól hydroxidu amonného a 2 mimimóly sírouhlíka. Výsledný katex je schopný zachycovat kovové ionty z roztoku.The present invention provides a process for preparing a dithiocarbamate cation exchanger group. This is how an anion containing, in particular, secondary amine the group in the active form is left 24 hours in aqueous ammonium hydroxide or alkali hydroxide to a pH of 7.5 to 9. After by filtration, the anion is washed with distilled water water and 1 millimeter of exchange capacity of anion exchange resin was added 1mM ammonium hydroxide and 2 mimimoles of carbon disulfide. The resulting cation exchanger is capable of trapping metal ions from solution.

Description

Vynález sa týká spósobu přípravy katexu s ditiokarbamátovou skupinou.The present invention relates to a process for preparing a cation exchange resin having a dithiocarbamate group.

V literatuře nie je popísaná příprava katexov tohoto typu, ani nie sú dostupné katexy tohoto typu.The preparation of cation exchangers of this type and cation exchangers of this type are not described in the literature.

Uvedený postup je popísaný v spósobe přípravy katexu s ditiokarbamátovou skupinou podfa vynálezu, ktorého podstatou je, že anex obsahujúci sekundárné aminové skupiny v aktívnej formě sa nechá napučať po dobu 24 hodin vo vodnom roztoku hydroxidu amonného alebo hydroxidu alkalického kovu pri hodnotě pH v rozmedzí 7,5 až 9,0. Po odfiltrovaní sa anex premyje destilovanou vodou do neutrálnej reakcie a na 1 milimól výmennej kapacity anexu sa přidá 1 milimól amoniaku vo formě vodného roztoku a 2 milimóly sírouhlíka.The process is described in a process for preparing a cation exchange resin having a dithiocarbamate group according to the invention, which comprises allowing the anion exchange resin containing the secondary amine groups in active form to swell for 24 hours in an aqueous solution of ammonium hydroxide or alkali metal hydroxide at pH 7. 5 to 9.0. After filtration, the anion exchanger is washed with distilled water until neutral and 1 millimole of anion exchange capacity is added with 1 millimole of ammonia in the form of an aqueous solution and 2 millimoles of carbon disulphide.

Výhodou spósobu podfa vynálezu je, že sa získá katetx s ditiokarbamátovou skupinou, ktorý má výhodné vlastnosti využitelné najma pri zachytávaní kovových iónov z roztoku. Výměnná rovnováha je posunutá v smere tvorby ditiokarbamátových komplexov kovov a preto je takýto ionex využitelný najma pre prekoncentráciu v stopovej analýze a dalej je možné ho využiť na čistenie niektorých elektrolytov od znečistenia niektorými kovovými iónami přítomnými v extrémně nízkých koncentráciach. Pri spósobe přípravy sa na organickom skeletu polymerného alebo polykondenzovaného typu obsahujúceho najma sekundárnu amínovú skupinu reakciou v mierne alkalickom prostředí syntetizuje pevne viazaná ditiokarbamátová skupina, ktorá má výhodné vlastnosti v súvislostl s viazaním — zachytáváním kovových iónov z roztoku, najma prvkov I., II., III. a IV. b podskupin periodického systému Mendelejeva. Připravený katex má úplné nové odlišné vlastnosti ako doteraz vyrábané ionexy.An advantage of the process according to the invention is that a dithiocarbamate group catheter is obtained which has advantageous properties useful, in particular, for trapping metal ions from solution. The exchange equilibrium is shifted in the direction of formation of the dithiocarbamate metal complexes, and therefore such an ion exchanger is particularly useful for preconcentration in trace analysis and further can be used to purify some electrolytes from contamination by some metal ions present in extremely low concentrations. In the method of preparation, a tightly bound dithiocarbamate group is synthesized on an organic backbone of a polymer or polycondensated type containing at least a secondary amine group by reaction in a mildly alkaline environment, which has advantageous properties in relation to binding - trapping of metal ions from solution, especially elements I, II. III. and IV. b subgroups of the Mendeleyev periodic system. The prepared cation exchanger has completely new, different properties than the ion exchangers produced hitherto.

Predmet vynálezu je ilustrovaný na příklade.The subject of the invention is illustrated by way of example.

Do kadičky objemu 250 ml sa odváži 30 g suchého anexu na báze polyetylénamínu s iónovýmennými skupinami primárnými, sekundárnými a terciárnymi. Jeho iónovýmenná kapacita je 10 milimólov na 1 g suroviny. (Wofalit L 150). Ďalej sa přidá 150 ml destilovanej vody. Vodným roztokom amoniaku o koncentrácii 5 % hmot. alebo hydroxidu sodného tej istej koncentrácie sa upraví pH roztoku na hodnotu 7,5 + 0,2 a za občasného miešania sa nechá anex napučať po dobu 24 hodin. Potom sa napučaný anex odfiltruje a premyje destilovanou vodou v objeme asi 2 1 (do neutrálnej reakcie filtrátu) pri laboratórnej teplote. Takto premytý anex sa vnesie do reakčnej banky, do ktorej sa přidá 100 ml destilovanej vody, 90 milimólov amoniaku v podobě 30 %-ného roztoku a za stálého miešania při laboratórnej teplote sa z deliacieho lievika po kvapkách rýchlosťou jedna kvapka za sekundu přidával 180 milimólov sírouhlíka. Reakčná zmes sa po ukončení pridávania sírouhlíka mieša ešte dve hodiny. Potom sa dekantáciou premýva připravený katex najmenej 6kráť 2 1 destilovanej vody. Takto připravený katex sa odfiltruje cez filtračný lievik a nechá sa na vzduchu v tenkej vrstvě vysušit pri teplote miestnosti 24 hodin.Weigh 30 g of dry anion exchange resin based on polyethylene amine with primary, secondary and tertiary ion exchange groups into a 250 ml beaker. Its ion exchange capacity is 10 millimoles per g of raw material. (Wofalit L 150). Next, 150 ml of distilled water are added. 5% w / w aqueous ammonia solution. or sodium hydroxide of the same concentration, adjust the pH of the solution to 7.5 ± 0.2 and allow the anion exchange resin to swell for 24 hours with occasional stirring. The swollen anion exchanger is then filtered off and washed with distilled water in a volume of about 2 liters (until the filtrate is neutral) at room temperature. The soaked anion exchanger is introduced into a reaction flask to which 100 ml of distilled water, 90 millimoles of ammonia 30% solution are added, and 180 millimoles of carbon disulphide are added dropwise at a rate of one drop per second from the separatory funnel while stirring at room temperature. . After the addition of carbon disulfide, the reaction mixture was stirred for two hours. The prepared cation exchanger is then washed by decanting at least 6 times with 2 l of distilled water. The cation exchanger thus prepared is filtered through a filter funnel and allowed to air dry in a thin layer at room temperature for 24 hours.

Množstvo viazaných ditiokarbamátových skupin sa vypočítá z prírastku obsahu síry v iónomeniči před a po syntéze ditiokarbamátovej skupiny. Takto vyrobený katex s ditiokarbamátovou skupinou má kapacitu vyjadrenú na ditiokarbamátovú skupinu 1 až 2 milimóly na 1 g suchého ionexu.The amount of bound dithiocarbamate groups is calculated by increasing the sulfur content of the ion exchanger before and after the synthesis of the dithiocarbamate group. The dithiocarbamate group cation exchanger so produced has a capacity per dithiocarbamate group of 1 to 2 millimoles per g of dry ion exchange resin.

Takto připravený katex s ditiokarbamátovou skupinou možno výhodné využiť na zníženie obsahov kovových iónov vo vodných roztokoch róznych elektrolytov i neelektrolytov.The dithiocarbamate cation exchanger thus prepared can be advantageously used to reduce the metal ion content in aqueous solutions of different electrolytes and nonelectrolytes.

Claims (1)

PREDMETSUBJECT Spósob přípravy katexu s ditiokarbamátovou skupinou vyznačujúci sa tým, že anex obsahujúci sekundárné aminové skupiny v aktívnej formě sa nechá napučať po dobu 24 hodin vo vodnom roztoku hydroxidu amónneho alebo hydroxidu alkalického kovuMethod for preparing a cation exchange resin with a dithiocarbamate group, characterized in that the anion exchange resin containing the secondary amine groups in active form is swollen for 24 hours in an aqueous solution of ammonium hydroxide or an alkali metal hydroxide YNÁLEZU pri hodnotě pH 7,5 až 9 a po odfiltrovaní sa anex premyje destilovanou vodou a potom sa na 1 milimól výmennej kapacity anexu přidá 1 milimól amoniaku vo formě vodného roztoku a 2 milimóly sírouhlíka.The mixture is filtered and the anion exchanger is washed with distilled water and then 1 millimole of anion exchange capacity is added with 1 millimole of ammonia in the form of an aqueous solution and 2 millimoles of carbon disulphide.
CS559783A 1983-07-26 1983-07-26 Cation resin preparation method with dithiocarbamate group CS238421B1 (en)

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