Purification of poly ether ketone ketone by centrifugal filtration
A method for the manufacture of polyether ketone ketone (PEKK), including the steps of: reacting 1,4-bis(4-phenoxybenzoylbenzene) and/or diphenylether with at least one difunctional aromatic acyl chloride, in a reaction solvent and in presence of a Lewis acid, to obtain a product mixture including a PEKK-Lewis acid complex; contacting the obtained product mixture with a protic solvent, so as to form a dispersion that includes a liquid phase including Lewis acid and a second phase, e.g., a solid phase, including PEKK; and separating the second phase from the liquid phase by centrifugal filtration, so as to recover a crude PEKK and a effluent containing Lewis acid, wherein step (iii) includes a step of centrifugal filtration.
1. A method for the manufacture of polyether ketone ketone (PEKK), comprising the steps of:
(i) reacting 1,4-bis(4-phenoxybenzoylbenzene) and/or diphenylether with at least one difunctional aromatic acyl chloride, in a reaction solvent and in presence of a Lewis acid, to obtain a product mixture comprising a PEKK-Lewis acid complex;
(ii) contacting the obtained product mixture with a protic solvent so as to form a dispersion that comprises a liquid phase comprising Lewis acid and a second phase comprising PEKK; and
(iii) separating the second phase of the dispersion from the liquid phase, so as to recover a crude PEKK and an effluent containing Lewis acid,
wherein step (iii) comprises a step of centrifugal filtration,
wherein the method comprises after step (iii) further one or more steps of washing the crude PEKK, and subjecting the resulting mixture to a further solid/liquid separation, wherein the one (or more) washing step is (are) performed in a centrifugal filtration device, without removing the crude PEKK between subsequent steps.
2. The method of claim 1 , wherein the at least one difunctional aromatic acyl chloride is selected from terephtalic acid chloride, isophtalic acid chloride and the mixtures thereof.
3. The method of claim 1 , wherein the reaction solvent is ortho-dichlorobenzene.
4. The method of claim 1 , wherein the Lewis acid is aluminum trichloride.
5. The method of claim 1 , wherein the protic solvent used in step (ii) is an aqueous solution, which has a pH of not more than 5.
6. The method of claim 1 , wherein said further one or more steps of washing the crude PEKK is carried out in an alcoholic aqueous solution.
7. The method of claim 1 , wherein said further one or more steps of washing the crude PEKK is carried out in water.
8. The method of claim 1 , wherein the steps of washing the crude PEKK, and subjecting the resulting mixture to a further solid/liquid separation comprise:
(iv) one or more steps of washing the crude PEKK in methanol, and subjecting the mixture obtained to a solid/liquid separation comprising a step of centrifugal filtration; and
(v) one or more steps of washing the PEKK obtained in the previous step in water, and subjecting the mixture obtained to a solid / liquid separation comprising a step of centrifugal filtration to obtain a purified PEKK.
9. The method of claim 1 , wherein the step of centrifugal filtration in step (iii) is performed at an acceleration rate of at least 500 g.
10. The method of claim 2 , wherein step (iii) and each subsequent washing step is performed for a duration of one hour or less.
11. The method of claim 1 , further comprising a subsequent step of drying the purified PEKK.
12. The method of claim 1 , wherein the crude PEKK is purified without using a complexing agent.
13. The method of claim 1 , wherein the purified PEKK contains less than 1000 ppm.
14. The method of claim 1 , wherein the effluent containing Lewis acid is recycled.