ABSTRACT:Polymerization process of poly(ether ketone) made of diphenyl ether (DPE) and isophthaloyl chloride (IPC) catalyzed by aluminum chloride in dichloroethane was characterized by 1 H NMR. The polymerization gave a precipitate of polymer/catalyst complex during the reaction. End-group analyses for polymer appeared as precipitate and oligomers stayed in the solution were carried out respectively after decomposition of the complex by treatment with methanol. Time dependence of the content of end groups showed that the oligomer of which molecular weight exceeded a critical value precipitated out independent of the functionality of the end groups, and further reaction proceeded in the precipitate as well as in the solution. Another approach to understand the reaction was carried out by direct 1 H NMR observation of the polymerization in an NMR sample tube. This experiment detected the molecular weight change of soluble oligomer in the reaction system at real time, and the results were consistent with those of isolated oligomers described above.KEY WORDS Poly(ether ketone) / Friedel-Crafts Acylation / End-Group Analysis / 1 H NMR / Polymer-Catalyst Complex / Precipitate / Poly(arylene ether ketone)s (PEKs) are well known as high performance semicrystalline polymers having excellent thermal stability, mechanical properties and solvent resistance.Preparations of PEKs are classified into two methods. [1][2][3] One is the aromatic nucleophilic substitution reaction between activated aromatic halides and alkali metal phenoxides in which ether linkages are formed. This method is used for the production of not only poly(ether ether ketone) (PEEK), most popular representative of PEKs, but also commercial polysulfones and poly(ether sulfone)s. The other method is the aromatic electrophilic substitution reaction between electron-rich aromatic hydrocarbons and aromatic acid chlorides in which ketone linkages are formed. This polymerization is carried out either in an organic solvent with aluminum chloride as a catalyst, 4, 5 FriedelCrafts acylation, or in hydrogen fluoride/boron trifluoride as a catalyst and solvent. 6, 7 The polymerization also includes dehydrative acylation reaction in polyphosphoric acid, 8,9 in trifluoromethanesulfonic acid 10 and in a methanesulfonic acid/phosphorus pentoxide medium. 11 Preparation of poly(ether ketone)s with FriedelCrafts acylation catalyzed by aluminum chloride in dichloroethane as a solvent can be carried out under moderate conditions, and is considered as a convenient method to obtain poly(ether ketone)s on a laboratory scale. Furthermore, various combinations of monomers afford a number of structures of polymers.The polymerization by Friedel-Crafts acylation gives a precipitate of the complex of polymer and catalyst in the course of polymerization. 12 It has been revealed that the molecular weight of PEK increases in the precipitate with reaction time. 13 Since it is generally thought that precipitation during polymerization terminates the chain growth, the increase in molecular ...

Misato AKIYAMA(Mem.), Hiroyasu SANO, Manabu OMORI Wireless power transfer that supply electric energy without wires is attracting the attention now. Many of the technologies use magnetic or electric field, but it have common problems that transmission efficiency depend on transmission distance. Therefore, we propose "sandwiched structure antenna" which having two pair of transmission antennas and reception antennas. Using the new structure, transmission efficiency can be made substantially constant inside a confined space.