PROCESS FOR THE PREPARATION OF HIGHLY PURIFIED, DIALKYDITHIOPHOSPHINIC COMPOUNDS
申请人:Rhodia, Inc.
公开号:EP2084168A2
公开(公告)日:2009-08-05
US7572931B2
申请人:——
公开号:US7572931B2
公开(公告)日:2009-08-11
US8796487B2
申请人:——
公开号:US8796487B2
公开(公告)日:2014-08-05
[EN] PROCESS FOR THE PREPARATION OF HIGHLY PURIFIED, DIALKYDITHIOPHOSPHINIC COMPOUNDS<br/>[FR] PROCESSUS POUR LA PRÉPARATION DE COMPOSÉS DIALKYLDITHIOPHOSPHINIQUES HAUTEMENT PURIFIÉS
申请人:RHODIA
公开号:WO2008051584A2
公开(公告)日:2008-05-02
[EN] An improved process for production of dialkyldithiophosphinic acid including sulfurizing a purified dialkylphosphinic acid by: reacting a hypophosphorous acid or salt with a stoichiometric excess of an alpha olefin in the presence of a free radical initiator to form a reaction product comprising monoalkylphosphinic acid and dialkylphosphinic acid; adding sufficient aqueous base to the reaction product to i) form the salts of the phosphinic acids, and ii) establish an aqueous phase and an organic phase, wherein a monoalkylphosphinic acid solubilizes into an aqueous phase; separating the organic phase from the aqueous phase; acidifying the organic phase and removing the olefin from the organic phase; isolating the purified dialkylphosphinic acid product; and sulfurizing the purified dialkylphosphinic acid product to form a dialkydithiophosphinic acid. The present invention also provides a process for preparing purified dialkylthiophosphinic chloride, and a process for preparing purified dialkylmonothiophosphinic acids. [FR] La présente invention concerne un processus amélioré pour la production d'acide dialkyldithiophosphinique consistant à sulfuriser un acide dialkylphosphinique purifié en procédant aux étapes consistant : à faire réagir un acide ou un sel hydrophosphoreux avec une oléfine alpha en excès stoehiométrique en présence d'un initiateur à radicaux libres pour constituer un produit de réaction comprenant de l'acide monoalkylphosphinique et de l'acide dialkylphosphinique ; à ajouter suffisamment d'une base aqueuse au produit de réaction pour i) former les sels des acides phosphiniques, et ii) établir une phase aqueuse et une phase organique, l'acide monoalkylphosphinique se solubilisant dans une phase aqueuse ; à séparer la phase organique de la phase aqueuse ; à acidifier la phase organique et à retirer l'oléfine de la phase organique, à isoler le produit d'acide dialkylphosphinique purifié ; et à sulfuriser le produit d'acide dialkylphosphinique purifié pour obtenir de l'acide dialkyldithiophosphinique. La présente invention concerne aussi un processus servant à préparer du chlorure dialkylthiophosphinique purifié, et un processus servant à préparer des acides dialkylmonothiophosphiniques purufiés.
Process for the preparation of highly purified, dialkydithiophosphinic compounds
申请人:Liu Leo Zhaoqing
公开号:US20080103330A1
公开(公告)日:2008-05-01
An improved process for production of dialkyldithiophosphinic acid including sulfurizing a purified dialkylphosphinic acid by: reacting a hypophosphorous acid or salt with a stoichiometric excess of an alpha olefin in the presence of a free radical initiator to form a reaction product comprising monoalkylphosphinic acid and dialkylphosphinic acid; adding sufficient aqueous base to the reaction product to i) form the salts of the phosphinic acids, and ii) establish an aqueous phase and an organic phase, wherein a monoalkylphosphinic acid solubilizes into an aqueous phase; separating the organic phase from the aqueous phase; acidifying the organic phase and removing the olefin from the organic phase; isolating the purified dialkylphosphinic acid product; and sulfurizing the purified dialkylphosphinic acid product to form a dialkydithiophosphinic acid. The present invention also provides a process for preparing purified dialkylthiophosphinic chloride, and a process for preparing purified dialkylmonothiophosphinic acids.