Method for liquid/liquid extraction of molecular weight fractions of perfluorinated polyethers
View Patent ↗A liquid/liquid extraction method is used for separating a perfluorinated polyether (PFPE) into two molecular-weight distributions using an alcohol or cyclic ether as one solvent and a fluorinated solvent as the other solvent. The more polar alcohol or cyclic ether solvent extracts the lower molecular weight PFPE and the less polar fluorinated solvent extracts the higher molecular weight PFPE. In addition, when the PFPE is a mixture of PFPEs with different end groups, such as a mixture of predominantly Z-Tetraol but with other PFPEs with Z-Dol end groups, there is an enrichment of the Z-Tetraol in the more polar solvent. The preferred PFPE is a mixture of PFPEs in as-purchased Z-Tetraol and the preferred solvents are methanol or trifluoroethanol as one solvent and a perfluorinated hydrocarbon, such as perfluorohexane, as the other solvent.
1. A method for separating a perfluorinated polyether (PFPE) having di-hydroxyl end groups from a mixture of a first PFPE having hydroxyl end groups and a second PFPE having di-hydroxyl end groups, each of the first and second PFPEs having a distribution of molecular weights in the mixture, the method comprising:
providing an alcohol solvent and a fluorinated solvent;
mixing the PFPE mixture with the solvents in a liquid/liquid extractor to concentrate lower-molecular-weight second PFPE in the alcohol solvent and first PFPE and higher-molecular-weight second PFPE in the fluorinated solvent;
after mixing, separating the solvents; and
evaporating the alcohol solvent to substantially isolate lower-molecular-weight second PFPE from the mixture.
2. The method of claim 1 wherein the alcohol is methanol.
3. The method of claim 1 wherein the alcohol is trifluoroethanol.
4. The method of claim 1 wherein the fluorinated solvent is selected from perfluorinated hydrocarbons, hydrochlorofluorocarbons, hydrofluoroethers, hydrofluorocarbons, hydrohalofluoroethers, perfluorinated amines and perfluorinated cyclic ether.
5. The method of claim 4 wherein the fluorinated solvent is a perfluorinated hydrocarbon.
6. The method of claim 5 wherein the fluorinated solvent is perfluorohexane.
7. The method of claim 1 wherein the second solvent is a mixture of a perfluorinated hydrocarbon or a perfluorinated cyclic ether with a hydrochlorofluorocarbon, a hydrofluoroether, a hydrofluorocarbon, or a hydrohalofluoroether.
8. The method of claim 1 wherein said second PFPE has the general structural formula:
R—CF 2 —O—(CF 2 O) m —(CF 2 —CF 2 —O) n —CF 2 —R
where m and n are integers and
R=—CH 2 OCH 2 CH(OH)CH 2 OH.
9. The method of claim 1 wherein each of the first and second PFPEs has the general structural formula:
R—CF 2 —O—(CF 2 O) m —(CF 2 —CF 2 —O) n —CF 2 —R
where m and n are integers, and where R=—CH 2 OH for the first PFPE, and
R=—CH 2 OCH 2 CH(OH)CH 2 OH for the second PFPE.