Name: synthesis of high purity nonsymmetric dialkylphosphinic acid extractants
Uploaded: 2017-10-19T12:30:00
Description: Watch this Scientific Journal Video about Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants at JoVE.com

Detta arbete stöds av den nationella natur Science Foundation i Kina (21301104), den grundläggande forskningsmedel för Central universiteten (FRF-TP-16-019A3), och den statliga nyckel laboratorium för kemiteknik (SKL-ChE-14A04).

1. syntes av Mono-(2,3-dimethylbutyl) phosphinic syra 18 , 19 <ol><li>reaktion <ol><li>väga 31,80 g natrium natriumhypofosfit hydrat, 16.00 g ättiksyra, 8,42 g 2,3-dimethyl-1-buten, 0,73 g di - tert-butylnperoxide (DTBP), 25.00 g tetrahydrofuran (THF) till en 100 mL Teflon-fodrade rostfritt stål autoklav, sätta en magnetomrörare i autoklav och försegla den.</li>
		<li>Sätta autoklav i ett vertikalt rör ugn som är en magneti...

<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>

Det mest kritiska steget inom protokollet är mono-alkylphosphinic acid syntesen (figur 1en). I denna reaktion är en högre avkastning och mindre dialkylphosphinic syra biprodukt bättre. Ökande molar förhållandet av NaH2PO2/olefin A kommer att förbättra avkastningen och hämma generationen av dialkylphosphinic syra biprodukt. Dock kommer en stor NaH2PO2 dosering också öka kostnaden och orsaka omrörning problem. Rekommende...

Sura fosfororganiska extraktionsmedel används allmänt i fältet traditionella hydrometallurgi för utvinning och separation av sällsynta jordartsmetaller joner1,2, icke-järnmetaller (som Co/Ni3,4), () sällsynta metaller såsom Hf/Zr5, V6,7), aktinider8, etc. Under de senaste åren, har de också uppmärksammats mer i fälten sekundär resurs återvinning och högaktivt flytande avfall9. Di-(2-etylhexyl) fosforsyra (D2EHPA eller P204), 2-ethylhexylphosphoric acid mono-2-etylhexylester (EHEHPA, PC 88A eller P507) och Di-(2,4, 4'-trimethylpentyl)-phosphinic syra (Cyanex272), som företrädare för dialkylphosphoric syror, respektive är alkylphosphoric syra mono-alkylestrar, och dialkylphosphinic syror den vanligaste extraktionsmedel. Deras syra minskar i följande ordning: P204 &#62; P507 &#62; Cyanex 272. Den motsvarande extraktion förmåga, utvinning kapacitet och stripp surhetsgrad är alla i storleksordningen P204 &#62; P507 &#62; Cyanex 272 och separation prestanda är i omvänd ordning. Dessa tre extraktionsmedel är effektiva i de flesta fall. Det finns dock fortfarande vissa förhållanden där de inte är så effektiv: i tunga sällsynta jordartsmetaller separation, som de befintliga huvudproblem är dålig selektivitet och hög stripp syra för P204 och P507, låg utvinning kapacitet och emulsion tendens under extraktionen för Cyanex 272. Således dragit utvecklingen av romanen extraktionsmedel större uppmärksamhet under senare år.
Klassen av dialkylphosphinic syra extraktionsmedel anses vara en av de viktigaste aspekterna för forskning att utveckla nya extraktionsmedel. Ny forskning visade att utvinning förmåga dialkylphosphinic syror beror till stor del på strukturera av alkyl substituent10,11. Det kan vara ett brett utbud från betydligt högre än för P507 till lägre än Cyanex 27212. Men är utforskningen av Roman dialkylphosphinic syra extraktionsmedel begränsat till kommersiella olefin struktur10,12,13,14,15, 16. Även om dialkylphosphinic syra extraktionsmedel kan också syntetiseras av metoden Grignard-reaktion, är reaktion villkor rigorösa12,17.
NSDAPA, varav de två alkyls är olika, öppnar en dörr till utforskandet av nya extraktionsmedel. Det gör strukturerna av dialkylphosphinic syra mångsidigare, och dess utvinning och separation prestanda går att fininställa genom att ändra båda dess alkyl strukturer. Den traditionella syntetiska metoden för NSDAPA används PH3 som fosfor, som har många nackdelar som hög toxicitet, rigorösa reaktionsbetingelser och svårt rening. Vi rapporterade nyligen en ny metod att syntetisera NSDAPA med natrium natriumhypofosfit eftersom fosfor källa (se figur 1) och framgångsrikt syntetiseras tre NSDAPAs18. Detta detaljerade protokoll kan hjälpa nya utövare upprepa experimenten och behärska den syntetiska metoden för NSDAPA extraktionsmedel. Vi tar (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic syra som ett exempel. Namn och strukturer av olefin A, mono-alkylphosphinic syran mellanliggande, olefin B och de motsvarande NSDAPA visas i tabell 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>
</table>

synthesis of high purity nonsymmetric dialkylphosphinic acid extractants

Vi presenterar syntesen av (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic syra som exempel att visa en metod för syntesen av hög renhet nonsymmetric dialkylphosphinic syra extraktionsmedel. Låg giftiga natrium natriumhypofosfit valdes som fosfor källa att reagera med olefin en (2,3-dimethyl-1-buten) att generera en monoalkylphosphinic syra mellanliggande. Amantadin har antagits för att ta bort den dialkylphosphinic syra biprodukt, som endast den monoalkylphosphinic syran kan reagera med amantadin att bilda en amantadine∙mono-alkylphosphinic acid salt, medan den dialkylphosphinic syran inte reagera med amantadin på grund dess stora sterisk hinder. Den rena monoalkylphosphinic syran var då reagerade med olefin B (diisobutylene) att ge nonsymmetric dialkylphosphinic syra (NSDAPA). Oreagerad monoalkylphosphinic syran lätt kan tas bort genom en enkel bas-syra efter behandling och andra organiska föroreningar kan skiljas ut genom utfällning av cobalt salt. Strukturera av den (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic syra bekräftades av 31P NMR, 1H NMR, ESI-MS och FT-IR. Renheten bestämdes genom en metod för Potentiometrisk titrering och resultaten tyder på att renheten kan överstiga 96%.

31 P NMR spectra samlades för mono-(2,3-dimethylbutyl) phosphinic syran före och efter rening av metoden amantadin (figur 1a-b). 31 P NMR spectra, 1H NMR spectra, MS spectra och FT-IR spectra samlades för (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic syra (se figur 3, bild 4, bild 5och f...

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Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants

Syntesen av hög renhet Nonsymmetric Dialkylphosphinic syra extraktionsmedel

Ett protokoll för syntesen av hög renhet nonsymmetric dialkylphosphinic syra extraktionsmedel presenteras, tar (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic syra som ett exempel.

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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