Additive manufactured carbon michael addition articles and method to make them
US-2018362784-A1 · Dec 20, 2018 · US
US10689475B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10689475-B2 |
| Application number | US-201916255992-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jan 24, 2019 |
| Priority date | Jul 20, 2012 |
| Publication date | Jun 23, 2020 |
| Grant date | Jun 23, 2020 |
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The invention relates to polyaryl ether ketones with low contents of residual materials, whether they are residual monomers or solvents of the synthetic process.
Opening claim text (preview).
The invention claimed is: 1. A polyaryl ether ketone with a residual solvent content of less than 100 ppm and a residual aromatic ether content of less than 1%, wherein the residual solvent has a water solubility of less than 0.05% at 25° C., wherein the polyaryl ether ketone is free from any residual alcohol. 2. The polyaryl ether ketone of claim 1 , wherein the residual aromatic ether has a molar mass less than 500 g·mol −1 . 3. The polyaryl ether ketone of claim 1 , wherein the polyaryl ether ketone has a thermal stability inducing less than 2% of variation in the viscosity measured according to standard ISO 307. 4. The polyaryl ether ketone of claim 1 , wherein the polyaryl ether ketone is a polyether ketone ketone (PEKK). 5. The polyaryl ether ketone of claim 4 , wherein the residual aromatic ether is 1,4-bis(4-phenoxybenzoyl)benzene. 6. The polyaryl ether ketone of claim 2 , wherein the residual solvent is ortho-dichlorobenzene. 7. A polyaryl ether ketone obtained by a process which comprises the following consecutive steps: a) placing one or more aromatic acid chlorides and one or more aromatic ethers in contact with a Lewis acid in a solvent which has a water solubility of less than 0.05% at 25° C. at a temperature of between −5 and +25° C., with stirring; b) carrying out a polymerization of the aromatic acid chlorides and aromatic ethers and completing the polymerization at a temperature of between 50 and 120° C. to provide a reaction mixture which includes a polyaryl ether ketone; c) placing the reaction mixture in contact with water in the absence of alcohol with stirring in the optional presence of acid to extract the Lewis acid, forming a mixture of polyaryl ether ketone and liquid effluents; d) separating the polyaryl ether ketone from the liquid effluents; e) performing azeotropic distillation on the polyaryl ether ketone so as to eliminate residual solvent; f) washing the polyaryl ether ketone; and g) drying the polyaryl ether ketone at a temperature above Tg+20° C.; wherein the polyaryl ether ketone has a residual solvent content of less than 100 ppm and a residual aromatic ether content of less than 1%. 8. The polyaryl ether ketone of claim 7 , wherein the polyaryl ether ketone has a thermal stability inducing less than 2% of variation in the viscosity measured according to standard ISO 307. 9. The polyaryl ether ketone of claim 7 , wherein the polyaryl ether ketone is a polyether ketone ketone (PEKK). 10. The polyaryl ether ketone of claim 9 , wherein the residual aromatic ether is 1,4-bis(4-phenoxybenzoyl)benzene. 11. The polyaryl ether ketone of claim 7 , wherein the residual solvent is ortho-dichlorobenzene. 12. The polyaryl ether ketone of claim 7 , wherein the polyaryl ether ketone is free from any residual alcohol.
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