Purification of 1,4-bis (4-phenoxybenzoyl)benzene by centrifugal filtration
View Patent ↗A method for manufacturing 1,4-bis(4-phenoxybenzoylbenzene), including: reacting terephthaloyl chloride with diphenyl ether in a reaction solvent and in the presence of a Lewis acid, so as to obtain a product mixture including a 1,4-bis(4-phenoxybenzoylbenzene)-Lewis acid complex; contacting the product mixture with a protic solvent, so as to obtain a first phase containing the Lewis acid and a second phase containing 1,4-bis(4-phenoxybenzoylbenzene); subjecting at least the second phase to a solid/liquid separation step by centrifugal filtration, so as to recover solid 1,4-bis(4-phenoxybenzoylbenzene).
1. A method for manufacturing 1,4-bis(4-phenoxybenzoylbenzene), comprising:
reacting terephthaloyl chloride with diphenyl ether in a reaction solvent and in the presence of a Lewis acid, so as to obtain a product mixture comprising a 1,4-bis(4-phenoxybenzoylbenzene)-Lewis acid complex;
contacting the product mixture with a protic solvent, so as to obtain a first phase containing the Lewis acid and a second phase containing 1,4-bis(4-phenoxybenzoylbenzene);
subjecting at least the second phase to a solid/liquid separation step by centrifugal filtration, so as to recover solid 1,4-bis(4-phenoxybenzoylbenzene).
2. The method of claim 1 , comprising one or more steps of washing the recovered solid 1,4-bis(4-phenoxybenzoylbenzene) in a protic solvent and subjecting it to a further solid/liquid separation.
3. The method of claim 2 , wherein at least one of the steps of washing the solid 1,4-bis(4-phenoxybenzoylbenzene) is performed at a temperature of at least 20° C.
4. The method of claim 2 , wherein each step of washing the recovered the solid 1,4-bis(4-phenoxybenzoylbenzene) is performed in a centrifugal filtration device.
5. The method of claim 1 , further comprising:
separating the first phase from the second phase; and/or
heating the second phase up to a maximum temperature, followed by cooling the second phase down to a separation temperature, before subjecting the second phase to the solid/liquid separation step.
6. The method of claim 5 , wherein from 30 to 99.9 wt. % of the 1,4-bis(4-phenoxybenzoylbenzene) contained in the second phase is dissolved in the second phase at the maximum temperature.
7. The method of claim 5 , wherein the maximum temperature is from 90 to 150° C.
8. The method of claim 5 , wherein the separation temperature is at least 20° C.
9. The method of claim 5 , wherein the second phase is cooled down at a rate of from 10 to 50° C./h.
10. The method of claim 1 , wherein the protic solvent that the product mixture is contacted with is an aqueous solution.
11. The method of claim 1 , wherein the product mixture is poured into a vessel containing the protic solvent.
12. The method of claim 1 , wherein the second phase is subjected to the solid/liquid separation step at a temperature of at least 20° C.
13. The method of claim 1 , wherein the Lewis acid is aluminum trichloride.
14. The method of claim 1 , wherein the reaction solvent is ortho-dichlorobenzene.
15. A method of making a polyether ketone ketone polymer, comprising:
manufacturing 1,4-bis(4-phenoxybenzoylbenzene) according to the method of claim 1 ;
reacting said 1,4-bis(4-phenoxybenzoylbenzene) with at least one difunctional aromatic acyl chloride.