FIELD: chemistry.
SUBSTANCE: described is a method of obtaining polyphenylene ether ketone oxymate, consisting in the interaction of dioxymate anions of 4,4'-diacetyldiphenyloxide with 4,4'-dihalogenbenzophenone at higher temperatures in the aprotonic dipolar solvent dimethylsulphoxide, characterised by the fact that the synthesis of polyphenylene ether ketone oxymate is carried out in two stages: at the first stage with the reaction of potassium dioxymate of 4,4'-diacetyldiphenyloxide with 4,4'-dichlorobenzophenone with a molar ratio of 1:0.5 and the concentration of a solution C=1 mol/l in terms of dioxymate for 1 hour at a temperature of 165°C in the presence of a solid powder-like KOH obtained is a dioxymate anion of the following structure -O-N=C(CH3)-C6H4-O-C6H4-C(CH3)=N-O-C6H4-CO-C6H4-O-N=C(CH3)-C6H4-O-C6H4-C(CH3)=N-O-, at the second terminating stage of the process a mixture of 4,4'-difluorobenzophenone, 4,4'-dichlorobenzophenone and crushed and annealed K2CO3 in molar ratios of 0.5:0.005:0.15, counted per 1 mol of the initial diketoxime of 4,4'-diacetyldiphenyloxide, in a water-free DMSO, with an additional volume of the water-free DMSO being taken in such an amount that the concentration of the solution by each of the monomers at the second oligopolymer stage of the synthesis becomes equal to 0.5 mol/l, the total time of carrying out the reaction is 6 hours at a temperature of 165°C.
EFFECT: intensification, optimisation and cheapening of the process of obtaining polyphenylene ether ketone oxymate.
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Authors
Dates
2015-01-10—Published
2013-07-02—Filed