Name: synthesis of high purity nonsymmetric dialkylphosphinic acid extractants
Uploaded: 2017-10-19T12:30:00
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Questo lavoro è stato supportato dalla nazionale natura Science Foundation of China (21301104), i fondi di ricerca fondamentali per le Università centrale (FRF-TP-16-019A3) e lo stato chiave laboratorio di ingegneria chimica (SKL--14A04).

1. sintesi di Mono-(2,3-dimethylbutyl) Acido fosfinico 18 , 19 <ol><li>reazione <ol><li>pesare 31,80 g idrato ipofosfito di sodio, ore 16.00 g di acido acetico, 8,42 g 2,3-dimetil-1-butene, 0,73 g di - tert-butylnperoxide (DTBP) e g 25,00 tetraidrofurano (THF) in autoclave a 100 mL in acciaio inox rivestito in Teflon, mettere un agitatore magnetico in autoclave e sigillare it.</li>
		<li>Mettere l'autoclave in un forno tubolare vert...

<ol>
	<li>Swain, B., Otu, E. O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Competitive+extraction+of+lanthanides+by+solvent+extraction+using+Cyanex+272:+Analysis,+classification+and+mechanism.">Competitive extraction of lanthanides by solvent extraction using Cyanex 272: Analysis, classification and mechanism.</a> Sep Purif Technol. 83, 82-90 (2011).</li><li>Wang, Y. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+novel+extraction+process+based+on+CYANEX+(R)+572+for+separating+heavy+rare+earths+from+ion-adsorbed+deposit.">The novel extraction process based on CYANEX (R) 572 for separating heavy rare earths from ion-adsorbed deposit.</a> Sep Purif Technol. 151, 303-308 (2015).</li><li>Regel-Rosocka, M., Staszak, K., Wieszczycka, K., Masalska, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Removal+of+cobalt(II)+and+zinc(II)+from+sulphate+solutions+by+means+of+extraction+with+sodium+bis(2,4,4-trimethylpentyl)phosphinate+(Na-Cyanex+272).">Removal of cobalt(II) and zinc(II) from sulphate solutions by means of extraction with sodium bis(2,4,4-trimethylpentyl)phosphinate (Na-Cyanex 272).</a> Clean Technol Envir. 18 (6), 1961-1970 (2016).</li><li>Hereijgers, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Separation+of+Co(II)/Ni(II)+with+Cyanex+272+using+a+flat+membrane+microcontactor:+Stripping+kinetics+study,+upscaling+and+continuous+operation.">Separation of Co(II)/Ni(II) with Cyanex 272 using a flat membrane microcontactor: Stripping kinetics study, upscaling and continuous operation.</a> Chem Eng Res Des. 111, 305-315 (2016).</li><li>Lee, M. S., Banda, R., Min, S. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Separation+of+Hf(IV)-Zr(IV)+in+H2SO4+solutions+using+solvent+extraction+with+D2EHPA+or+Cyanex+272+at+different+reagent+and+metal+ion+concentrations.">Separation of Hf(IV)-Zr(IV) in H2SO4 solutions using solvent extraction with D2EHPA or Cyanex 272 at different reagent and metal ion concentrations.</a> Hydrometallurgy. 152, 84-90 (2015).</li><li>Noori, M., Rashchi, F., Babakhani, A., Vahidi, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Selective+recovery+and+separation+of+nickel+and+vanadium+in+sulfate+media+using+mixtures+of+D2EHPA+and+Cyanex+272.">Selective recovery and separation of nickel and vanadium in sulfate media using mixtures of D2EHPA and Cyanex 272.</a> Sep Purif Technol. 136, 265-273 (2014).</li><li>Li, X. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermodynamics+and+mechanism+of+vanadium(IV)+extraction+from+sulphate+medium+with+D2EHPA,+EHEHPA+and+CYANEX+272+in+kerosene.">Thermodynamics and mechanism of vanadium(IV) extraction from sulphate medium with D2EHPA, EHEHPA and CYANEX 272 in kerosene.</a> Trans Nonferrous Met Soc China. 22 (2), 461-466 (2012).</li><li>Das, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+the+nature+of+organophosphorous+acid+moiety+on+co-extraction+of+U(VI)+and+mineral+acid+from+aqueous+solutions+using+D2EHPA,+PC88A+and+Cyanex+272.">Effect of the nature of organophosphorous acid moiety on co-extraction of U(VI) and mineral acid from aqueous solutions using D2EHPA, PC88A and Cyanex 272.</a> Hydrometallurgy. 152, 129-138 (2015).</li><li>Baba, A. A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Extraction+of+copper+from+leach+liquor+of+metallic+component+in+discarded+cell+phone+by+Cyanex+(R)+272.">Extraction of copper from leach liquor of metallic component in discarded cell phone by Cyanex (R) 272.</a> JESTEC. 11 (6), 861-871 (2016).</li><li>Du, R. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microwave-assisted+synthesis+of+dialkylphosphinic+acids+and+a+structure-reactivity+study+in+rare+earth+metal+extraction.">Microwave-assisted synthesis of dialkylphosphinic acids and a structure-reactivity study in rare earth metal extraction.</a> RSC Adv. 5 (126), 104258-104262 (2015).</li><li>Du, R. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=alpha,+beta-Substituent+effect+of+dialkylphosphinic+acids+on+anthanide+extraction.">alpha, beta-Substituent effect of dialkylphosphinic acids on anthanide extraction.</a> RSC Adv. 6 (61), 56004-56008 (2016).</li><li>Wang, J. L., Xu, S. X., Li, L. Y., Li, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+organic+phosphinic+acids+and+studies+on+the+relationship+between+their+structure+and+extraction-separation+performance+of+heavy+rare+earths+from+HNO3+solutions.">Synthesis of organic phosphinic acids and studies on the relationship between their structure and extraction-separation performance of heavy rare earths from HNO3 solutions.</a> Hydrometallurgy. 137, 108-114 (2013).</li><li>Hino, A., Nishihama, S., Hirai, T., Komasawa, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Practical+study+of+liquid-liquid+extraction+process+for+separation+of+rare+earth+elements+with+bis+(2-ethylhexyl)+phosphinic+acid.">Practical study of liquid-liquid extraction process for separation of rare earth elements with bis (2-ethylhexyl) phosphinic acid.</a> J Chem Eng Jpn. 30 (6), 1040-1046 (1997).</li><li>Ju, Z. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+extraction+performance+of+di-decylphosphinic+acid.">Synthesis and extraction performance of di-decylphosphinic acid.</a> Chin J Nonferrous Met. 20 (11), 2254-2259 (2010).</li><li>Li, L. Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dialkyl+phosphinic+acids:+Synthesis+and+applications+as+extractant+for+nickel+and+cobalt+separation.">Dialkyl phosphinic acids: Synthesis and applications as extractant for nickel and cobalt separation.</a> Trans Nonferrous Met Soc China. 20, 205-210 (2010).</li><li>Wang, J. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvent+extraction+of+rare+earth+ions+from+nitrate+media+with+new+extractant+di-(2,3-dimethylbutyl)-phosphinic+acid.">Solvent extraction of rare earth ions from nitrate media with new extractant di-(2,3-dimethylbutyl)-phosphinic acid.</a> J Rare Earths. 34 (7), 724-730 (2016).</li><li>Hu, W. X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+properties+of+di-tertiary+alkylphosphinic+acids.">Synthesis and properties of di-tertiary alkylphosphinic acids.</a> Chem J Chin Univ-Chin. 15 (6), 849-853 (1994).</li><li>Wang, J. L., Chen, G., Xu, S. M., Li, L. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+novel+nonsymmetric+dialkylphosphinic+acid+extractants+and+studies+on+their+extraction-separation+performance+for+heavy+rare+earths.">Synthesis of novel nonsymmetric dialkylphosphinic acid extractants and studies on their extraction-separation performance for heavy rare earths.</a> Hydrometallurgy. 154, 129-136 (2015).</li><li>Wang, J. L., Xie, M. Y., Wang, H. J., Xu, S. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvent+extraction+and+separation+of+heavy+rare+earths+from+chloride+media+using+nonsymmetric+(2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic+acid.">Solvent extraction and separation of heavy rare earths from chloride media using nonsymmetric (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid.</a> Hydrometallurgy. 167, 39-47 (2017).</li><li>Menoyo, B., Elizalde, M. P., Almela, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+the+degradation+compounds+formed+by+the+oxidation+of+thiophosphinic+acids+and+phosphine+sulfides+with+nitric+acid.">Determination of the degradation compounds formed by the oxidation of thiophosphinic acids and phosphine sulfides with nitric acid.</a> Anal Sci. 18 (7), 799-804 (2002).</li><li>Darvishi, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synergistic+effect+of+Cyanex+272+and+Cyanex+302+on+separation+of+cobalt+and+nickel+by+D2EHPA.">Synergistic effect of Cyanex 272 and Cyanex 302 on separation of cobalt and nickel by D2EHPA.</a> Hydrometallurgy. 77, 227-238 (2005).</li></ol>

Il punto più critico all'interno del protocollo è la sintesi mono-alkylphosphinic acido (Figura 1a). In questa reazione, un rendimento più elevato e meno sottoprodotto di acido dialkylphosphinic è meglio. Aumentando il rapporto molare di NaH2PO2/olefin A migliorerà il rendimento e inibire la generazione di sottoprodotto acido dialkylphosphinic. Tuttavia, un dosaggio elevato di NaH2PO2 sarà anche aumentare il costo e causare u...

Acidi solventi organofosforici sono ampiamente usati nel campo tradizionale Idrometallurgia per estrazione e separazione delle terre rare ioni1,2, metalli non ferrosi (come Co/Ni3,4), metalli rari ( ad esempio Hf/Zr5, V6,7), attinidi8, ecc. Negli ultimi anni, hanno anche attirato più attenzione nei campi della risorsa secondaria riciclaggio e smaltimento dei rifiuti liquidi ad alto livello9. Di-(2-etilesile) (D2EHPA o P204), 2-ethylhexylphosphoric acid mono-2-etilesil estere dell'acido fosforico (EHEHPA, PC 88A o P507) e Di-(2,4, 4'-trimethylpentyl)-Acido fosfinico (Cyanex272), che sono rappresentanti di acidi dialkylphosphoric, alchilfosforici acido mono-alchil esteri e acidi dialkylphosphinic rispettivamente, sono i solventi più comunemente usati. Loro acidità diminuisce nella seguente sequenza: P204 &#62; P507 &#62; Cyanex 272. La corrispondente capacità di estrazione, capacità di estrazione e stripping acidità sono tutti in ordine P204 &#62; P507 &#62; Cyanex 272 e le prestazioni di separazione è nell'ordine opposto. Questi tre solventi sono efficaci nella maggior parte dei casi. Tuttavia, ci sono ancora alcune condizioni dove non sono così efficienti: nella separazione di terre rare pesanti, di cui i principali problemi esistenti sono la scarsa selettività ed elevata acidità stripping per P204 e P507, bassa capacità di estrazione e tendenza di emulsione durante l'estrazione per Cyanex 272. Così, lo sviluppo di nuovi solventi ha attirato maggiore attenzione negli ultimi anni.
La classe di solventi acidi dialkylphosphinic è considerata uno degli aspetti più importanti di ricerca per sviluppare nuovi solventi. Recenti ricerche hanno dimostrato che la capacità di estrazione di acidi dialkylphosphinic dipende in gran parte dalla struttura del alchile sostituenti10,11. Può essere una vasta gamma da significativamente superiore a quello di P507 inferiore a quella di Cyanex 27212. Tuttavia, l'esplorazione di solventi acidi dialkylphosphinic romanzo è limitato per le olefine commerciale struttura10,12,13,14,15, 16. Anche se dialkylphosphinic acidi solventi possono anche essere sintetizzato dal metodo reazione di Grignard, le condizioni di reazione sono rigorosi12,17.
NSDAPA, di cui i due alchili sono diversi, si apre una porta all'esplorazione di nuovi solventi. Rende le strutture di dialkylphosphinic acido più diversificata e sua estrazione e separazione delle prestazioni possono essere ottimizzata modificando sia delle sue strutture di alchile. Il tradizionale metodo sintetico di NSDAPA usato PH3 come una fonte di fosforo, che ha molti svantaggi come alta tossicità, condizioni di reazione rigorosa e difficile purificazione. Recentemente abbiamo segnalato un nuovo metodo per sintetizzare usando ipofosfito di sodio come un fosforo origine (vedere Figura 1) e sintetizzato con successo tre NSDAPAs18NSDAPA. Questo protocollo dettagliato può aiutare nuovi praticanti ripetere gli esperimenti e padroneggiare il metodo sintetico di solventi NSDAPA. Prendiamo (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico come un esempio. I nomi e le strutture di olefine A, l'acido mono-alkylphosphinic intermedio, olefine B e la corrispondente NSDAPA sono riportati nella tabella 1.

<table style="border-collapse:collapse;width:687pt" width="916">
	<colgroup>
		<col style="width:185pt" width="247" />
		<col style="width:290pt" width="387" />
		<col style="width:93pt" width="124" />
		<col style="width:119pt" width="158" />
	</colgroup>
	<tbody>
		<tr height="102" style="height:76.5pt">
			<td class="xl17" height="102" style="width:185pt;height:76.5pt" width="247">sodium hypophosphite hydrate</td>
			<td class="xl17" style="width:290pt" width="387">Tianjin Fuchen Chemical Reagents Factory</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: NaH2PO2&#8729;H2O, purity &#8805;99.0%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">2,3-dimethyl-1-butene</td>
			<td class="xl17" style="width:290pt" width="387">Adamas Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C6H12, purity &#8805;99%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">diisobutylene</td>
			<td class="xl17" style="width:290pt" width="387">Shanghai&#160;Aladdin&#160;Bio-Chem&#160;Technology&#160;Co.,&#160;LTD</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C8H16, purity 97%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">acetic acid</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C2H4O2, purity &#8805;99.5%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">di-tert-butylnperoxide</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C8H18O2, purity &#8805;97.0%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">tetrahydrofuran</td>
			<td class="xl17" style="width:290pt" width="387">Beijing Chemical Works</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C4H8O, purity A.R.</td>
		</tr>
		<tr height="102" style="height:76.5pt">
			<td class="xl17" height="102" style="width:185pt;height:76.5pt" width="247">amantadine hydrochloride</td>
			<td class="xl17" style="width:290pt" width="387">Shanghai&#160;Aladdin&#160;Bio-Chem&#160;Technology&#160;Co.,&#160;LTD</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C10H17N&#8729;HCl, purity 99%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">ethyl ether</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C4H10O, purity &#8805;99.7%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">ethyl acetate</td>
			<td class="xl17" style="width:290pt" width="387">Xilong Chemical Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C4H8O2, purity &#8805;99.5%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">acetone</td>
			<td class="xl17" style="width:290pt" width="387">Beijing Chemical Works</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C3H6O, purity &#8805;99.5%</td>
		</tr>
		<tr height="75" style="height:56.25pt">
			<td class="xl17" height="75" style="width:185pt;height:56.25pt" width="247">sodium hydroxide</td>
			<td class="xl17" style="width:290pt" width="387">Xilong Chemical Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: NaOH, purity &#8805;96.0%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">concentrated sulfuric acid</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: H2SO4, purity 95-98%</td>
		</tr>
		<tr height="75" style="height:56.25pt">
			<td class="xl17" height="75" style="width:185pt;height:56.25pt" width="247">hydrochloric acid</td>
			<td class="xl17" style="width:290pt" width="387">Beijing Chemical Works</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: HCl, purity 36-38%</td>
		</tr>
		<tr height="75" style="height:56.25pt">
			<td class="xl17" height="75" style="width:185pt;height:56.25pt" width="247">sodium chloride</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: NaCl, purity &#8805;99.5%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">anhydrous magnesium sulfate</td>
			<td class="xl17" style="width:290pt" width="387">Tianjin Jinke Institute of Fine Chemical Industry</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: MgSO4, purity &#8805;99.0%</td>
		</tr>
		<tr height="103" style="height:77.25pt">
			<td class="xl19" height="103" style="width:185pt;height:77.25pt" width="247">Cobalt(II) chloride hexahydrate</td>
			<td class="xl19" style="width:290pt" width="387">Xilong Chemical Co., Ltd.</td>
			<td class="xl19" style="width:93pt" width="124"></td>
			<td class="xl19" style="width:119pt" width="158">Molecular formula: CoCl2&#8729;6H2O, purity &#8805;99.0%</td>
		</tr>
	</tbody>
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synthesis of high purity nonsymmetric dialkylphosphinic acid extractants

Vi presentiamo la sintesi di (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico come esempio per illustrare un metodo per la sintesi di elevata purezza il dialkylphosphinic acido solventi. Ipofosfito di sodio basso tossico è stato scelto come la fonte di fosforo a reagire con olefine un (2,3-dimetil-1-butene) per generare un acido monoalkylphosphinic intermedio. L'amantadina è stata adottata per rimuovere il sottoprodotto di acido dialkylphosphinic, come solo l'acido monoalkylphosphinic può reagire con amantadina per formare un sale acido di amantadine∙mono-alkylphosphinic, mentre l'acido dialkylphosphinic non può reagire con amantadina a causa sua grande impedimento sterico. L'acido purificato monoalkylphosphinic quindi è stato reagito con olefine B (diisobutylene) per produrre il dialkylphosphinic acido (NSDAPA). L'acido non reagito monoalkylphosphinic possa essere facilmente rimossi con un semplice post-trattamento base-acido e altre impurità organiche possono essere separati attraverso la precipitazione del sale di cobalto. La struttura della (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico è stata confermata dalla RMN 31P, 1H NMR, ESI-MS e FT-IR. La purezza è stata determinata con un metodo di titolazione potenziometrica, ed i risultati indicano che la purezza può superare i 96%.

31 Gli spettri RMN P sono stati raccolti per l'acido fosfinico mono-(2,3-dimethylbutyl) prima e dopo la purificazione dal metodo amantadina (Figura 1a-b). 31 Gli spettri RMN P, spettri di 1H NMR, MS spettri e spettri FT-IR sono stati raccolti per (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico (vedere Figura 3, Figura 4, <strong class="x...

Watch this Scientific Journal Video about Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants at JoVE.com

Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants

Sintesi di elevata purezza il Dialkylphosphinic acido solventi

Un protocollo per la sintesi di elevata purezza il dialkylphosphinic acido solventi è presentato, prendendo (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico come un esempio.

We present the synthesis of (2,3-dimethylbutyl)(2,4,4&#39;-trimethylpentyl)phosphinic acid as an example to demonstrate a method for the synthesis of high ...

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