Polyether, polyester and polyether ester purification process

Details Polyether, polyester and polyether ester purification process Polyether, polyester and polyether ester purification process

1997-08-04

1998-10-20

Acquah, Samuel A.

Synthetic resins or natural rubbers -- part of the class 520 ser

Synthetic resins

Treating polymer containing material or treating a solid...

528482, 528487, 528488, 528489, 528490, 528491, 528502, 528503, 210767, 210768, C08F 600

Patent

active

058247696

DESCRIPTION:

BRIEF SUMMARY
The invention relates to a process for purifying heteropoly compound-containing polyethers, polyesters and polyether esters or their solutions by mixing the same with a compound which contains at least one heteroatom, which can be present as the central atom of a heteropolymer compound, is non-protic and is of a polarity so low that its addition leads to the separation of the heteropolymer compound in a separate phase.
Polyethers, polyesters and polyether esters are used in many ways; examples are their use in hydraulic oils or as diol component in the preparation of polyurethanes. These compounds are prepared by cationic polymerization or copolymerization of corresponding monomers, for example cyclic ethers, acetates, polyalcohols or lactones, using Bronsted acid or Lewis acid catalysts. Heteropolyacids and heteropolyacid salts, jointly termed "heteropoly compound(s)" or "HPA" below, have proved to be particularly advantageous catalysts for ring-opening polymerization. To establish the desired polymer molar mass and/or to prepare special end-group-modified derivatives, substances are customarily present in the polymerization whose inclusion leads directly or indirectly to chain termination. Examples of these are carboxylic acid derivatives, alcohols or water.
JP-A-33 028/1983 describes, for example, the polymerization of tetrahydrofuran (THF) in the presence of a carboxylic anhydride or carboxylic acid halide with the formation of polyTHF diesters, a heteropolyacid being used as catalyst.
EP 126 471 teaches the HPA-catalyzed polymerization of THF and the copolymerization of THF with various other cyclic ethers in the presence of water, with the formation of poly(ether glycols). EP 158 229 describes the preparation of poly(ether glycols) by copolymerization of cyclic ethers with di- and higher-functional alcohols.
According to JP 61-200120, lactones, or lactones together with cyclic ethers, can be polymerized in the presence of hydroxyl-containing compounds with heteropolyacids as catalysts.
Poly(ether glycol)monoethers and poly(ether glycol)monoesters may be prepared according to EP 503 393 and EP 503 394 by polymerizing cyclic ethers in the presence of monoalcohols or monocarboxylic acids with HPA catalysts.
In these polymerization processes for preparing polyethers, polyesters and polyether esters, polymer phases are formed which, on account of the incomplete conversion, still contain residual amounts of monomer(s) residual amounts of the compound(s) leading to chain termination, any solvents used, and also dissolved heteropoly compound(s). The percentage of HPA catalyst dissolved in the polymer phase is considerable in these reactions and can be up to 1% by weight or more, based on the polymer phase. The dissolved catalyst does not precipitate out in the event of a separation which merely consists of distilling off unreacted monomer, chain-termination reagent(s), and any solvent used, from this phase, but remains in dissolved form in the polymer. On the one hand, this must be prevented for quality reasons, and on the other hand it is desirable for reasons of costs, since heteropolyacids are very expensive, to recover the majority of the catalyst.
It is further known that heteropoly compounds decompose in the course of time, more intensively under thermal stress. This occurs principally by hydrolysis, with formation of the corresponding oxides. The decomposition of heteropoly compounds can be decreased or completely prevented if compounds are added which contain elements which can occur as central atoms in heteropoly compounds. For example, the hydrolytic stability of phosphorus poly acids is markedly increased in the presence of phosphoric acid (A. Aoshima, S. Yamamatsu, T. Yamaguchi, Nippon Kagaku Kaishi, (1990) 233). The hydrolytic stability of HPA is likewise increased under reducing conditions (M. T. Pope, E. Papaconstantinou, Inorg. Chem. 6 (1967) 1147).
To solve the problem of separating off heteropoly compounds, it is proposed in EP 181 621 to add a hydrocarbon or halogenated hydrocarbon to the

REFERENCES:
patent: 4677231 (1987-06-01), Aoshima et al.
patent: 5414143 (1995-05-01), Weyer et al.

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