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NMR study of the synthesis of Di 2-ethylhexylphosphoric acid with P{sub 4}O{sub 10}; Etude de la synthese de l`acide Di 2-ethylhexylphosphorique a partir de P{sub 4}O{sub 10} par resonnance magnetique nucleaire

Abstract

Various aspects of Di 2-ethylhexylphosphoric acid (DEHPA) synthesis were investigated using {sup 1}H, {sup 13}C and {sup 31}P NMR techniques. The first step of the present work consists of the identification and the determination of DEHPA, its derivatives and other intermediates in the reaction mixture without previous separation or purification. The second step is devoted to the study of the effects of the main factors, i.e. the reaction temperature, ROH/P{sub 2}O{sub 5} mole ratio, the reaction time and the presence of some additives upon the reaction. The spectra and the distribution of the reaction products were also discussed. As an important conclusion which can be withdrawn from the present investigations one can suggest that the -26 ppm triplet is due to the presence of triphosphorus compounds. Such compounds should result from the direct interaction between 2-ethylhexanol and the polymeric phosphorus anhydride during the first 40 minutes after the beginning of the reaction. Pyrophosphates i.e. diphosphorus intermediates and the monoester which exhibit a relatively higher stability were also yielded.
Authors:
Elias, A; Azouz, A; [1]  Rodehueser, L [2] 
  1. Centre de Developpement des Materiaux, Algiers (Algeria). Lab. de Synthese Organique
  2. Nancy Univ., 54 (France). Lab. de Chimie Physique Organique
Publication Date:
Dec 01, 1991
Product Type:
Technical Report
Report Number:
CDM/LSO-40; MDRTE-CDM-22.
Reference Number:
SCA: 400201; 360601; PA: AIX-23:018470; SN: 92000664343
Resource Relation:
Other Information: PBD: Dec 1991
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 36 MATERIALS SCIENCE; HDEHP; NMR SPECTRA; NUCLEAR MAGNETIC RESONANCE; CHEMICAL PREPARATION; CHEMICAL REACTIONS; ESTERS; ORGANIC PHOSPHORUS COMPOUNDS; 400201; 360601; CHEMICAL AND PHYSICOCHEMICAL PROPERTIES; PREPARATION AND MANUFACTURE
OSTI ID:
10121538
Research Organizations:
Centre de Developpement des Materiaux, Algiers (Algeria). Lab. de Synthese Organique
Country of Origin:
Algeria
Language:
French
Other Identifying Numbers:
Other: ON: DE92617561; TRN: DZ9100071018470
Availability:
OSTI; NTIS (US Sales Only); INIS
Submitting Site:
INIS
Size:
32 p.
Announcement Date:
Jun 30, 2005

Citation Formats

Elias, A, Azouz, A, and Rodehueser, L. NMR study of the synthesis of Di 2-ethylhexylphosphoric acid with P{sub 4}O{sub 10}; Etude de la synthese de l`acide Di 2-ethylhexylphosphorique a partir de P{sub 4}O{sub 10} par resonnance magnetique nucleaire. Algeria: N. p., 1991. Web.
Elias, A, Azouz, A, & Rodehueser, L. NMR study of the synthesis of Di 2-ethylhexylphosphoric acid with P{sub 4}O{sub 10}; Etude de la synthese de l`acide Di 2-ethylhexylphosphorique a partir de P{sub 4}O{sub 10} par resonnance magnetique nucleaire. Algeria.
Elias, A, Azouz, A, and Rodehueser, L. 1991. "NMR study of the synthesis of Di 2-ethylhexylphosphoric acid with P{sub 4}O{sub 10}; Etude de la synthese de l`acide Di 2-ethylhexylphosphorique a partir de P{sub 4}O{sub 10} par resonnance magnetique nucleaire." Algeria.
@misc{etde_10121538,
title = {NMR study of the synthesis of Di 2-ethylhexylphosphoric acid with P{sub 4}O{sub 10}; Etude de la synthese de l`acide Di 2-ethylhexylphosphorique a partir de P{sub 4}O{sub 10} par resonnance magnetique nucleaire}
author = {Elias, A, Azouz, A, and Rodehueser, L}
abstractNote = {Various aspects of Di 2-ethylhexylphosphoric acid (DEHPA) synthesis were investigated using {sup 1}H, {sup 13}C and {sup 31}P NMR techniques. The first step of the present work consists of the identification and the determination of DEHPA, its derivatives and other intermediates in the reaction mixture without previous separation or purification. The second step is devoted to the study of the effects of the main factors, i.e. the reaction temperature, ROH/P{sub 2}O{sub 5} mole ratio, the reaction time and the presence of some additives upon the reaction. The spectra and the distribution of the reaction products were also discussed. As an important conclusion which can be withdrawn from the present investigations one can suggest that the -26 ppm triplet is due to the presence of triphosphorus compounds. Such compounds should result from the direct interaction between 2-ethylhexanol and the polymeric phosphorus anhydride during the first 40 minutes after the beginning of the reaction. Pyrophosphates i.e. diphosphorus intermediates and the monoester which exhibit a relatively higher stability were also yielded.}
place = {Algeria}
year = {1991}
month = {Dec}
}