FIELD: chemical processes.
SUBSTANCE: invention relates to a method for synthesising polyaryletherketones (PEKK) which can be applied as structural materials. Proposed method includes the stages of: a) producing 1,3-bis(4-phenoxybenzoyl)benzene (1,3-EKKE); b) mixing terephthalic acid dichloride (TPC) and benzoyl chloride (BC) with the 1,3-EKKE produced at stage (a) in an aprotic solvent, resulting in a reaction solution wherein the water content in the aprotic solvent is from 1 to 100 ppm; c) adding a Lewis acid to the reaction solution as a catalyst, wherein the catalyst is added at a temperature from -30 to 10°C, resulting in a reaction mixture; d) heating the reaction mixture formed at stage (c) to the reaction temperature; e) sustaining the reaction mixture formed at stage (c), resulting in a PEKK-containing product mixture; f) isolating solid PEKK by consecutively washing an inorganic acid in the aqueous solution; g) removing the residual content of inorganic acid in the aqueous solution of a neutralising agent, followed by filtering; h) purifying the resulting solid PEKK by washing, followed by filtering, resulting in crude PEKK; i) drying the resulting crude PEKK, resulting in a target PEKK with a characteristic viscosity of the solution in concentrated H2SO4 of 1.02±0.05 dl/g. The method for producing 1,3-EKKE therein includes: a) mixing isophthalic acid dichloride (IPC) and diphenyl ether (DPE) with an aprotic solvent, resulting in a reaction solution, wherein the water content in the aprotic solvent is from 1 to 100 ppm; b) adding a Lewis acid to the reaction solution as a catalyst, wherein the catalyst is added at a temperature of -30 to 10°C, resulting in a reaction mixture; c) heating the reaction mixture to the reaction temperature from 10 to 40°C; d) sustaining the reaction mixture at the reaction temperature, resulting in a 1,3-EKKE-containing product mixture; e) isolating raw 1,3-EKKE by deactivating the 1,3-EKKE-containing product mixture with a proton solvent; f) purifying the raw 1,3-EKKE by recrystallisation, followed by filtering; drying the resulting solid 1,3-EKKE.
EFFECT: production of PEKK with better recyclability and a reduced amount of xanthohydrol groups, the characteristic viscosity of the solution whereof in concentrated sulphuric acid is from 0.97 to 1.07 cm3/g; wherein the complex dynamic viscosity of the polymer melt varies insignificantly throughout a long time interval (up to 45 minutes) and ranges from 500 to 1,750 Pa·s.
35 cl, 3 dwg, 1 tbl, 10 ex
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Authors
Dates
2022-07-05—Published
2020-12-30—Filed