Method of forming phenylene ether oligomer
US-2018362430-A1 · Dec 20, 2018 · US
US10059802B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10059802-B2 |
| Application number | US-201715465812-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 22, 2017 |
| Priority date | Mar 28, 2016 |
| Publication date | Aug 28, 2018 |
| Grant date | Aug 28, 2018 |
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Provided is a method for producing polyphenylene ether (PPE) having excellent mechanical properties, heat aging resistance, and color, and in which the content of impurities such as low molecular weight components and catalyst metal is low. The method for producing PPE includes: performing oxidative polymerization of a phenolic compound in a polymerization solution containing the phenolic compound, a catalyst, and an aromatic solvent to obtain a PPE mixed liquid; precipitating PPE to obtain a slurry containing particulate PPE through addition of a polar solvent to the PPE mixed liquid; solid-liquid separating the slurry to obtain wet PPE particles; washing the wet PPE particles to obtain PPE particles through at least one cycle of a washing and solid-liquid separation process in which washing is performed with a washing liquid containing an aromatic solvent and a polar solvent, and in which solid-liquid separation is performed; and drying the PPE particles.
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The invention claimed is: 1. A method for producing polyphenylene ether comprising: performing oxidative polymerization of a phenolic compound in a polymerization solution containing the phenolic compound, a catalyst, and at least one aromatic solvent selected from the group consisting of benzene, toluene, xylene, and ethylbenzene to obtain a polyphenylene ether mixed liquid; precipitating polyphenylene ether to obtain a slurry containing particulate polyphenylene ether by adding, to the polyphenylene ether mixed liquid, at least one polar solvent selected from the group consisting of water, a ketone having a carbon number of 1-10, and an alcohol having a carbon number of 1-10; solid-liquid separating the slurry to obtain wet polyphenylene ether particles; performing a washing and solid-liquid separation process by washing the wet polyphenylene ether particles with a washing liquid containing at least one aromatic solvent selected from the group consisting of benzene, toluene, xylene, and ethylbenzene and at least one polar solvent selected from the group consisting of water, a ketone having a carbon number of 1-10, and an alcohol having a carbon number of 1-10, and solid-liquid separating the polyphenylene ether particles and the washing liquid to obtain polyphenylene ether particles; and drying the polyphenylene ether particles. 2. The method for producing polyphenylene ether of claim 1 , wherein the washing and solid-liquid separation process are performed for at least two cycles. 3. The method for producing polyphenylene ether of claim 2 , wherein in a final cycle of the washing and solid-liquid separation process, the polyphenylene ether particles are obtained by solid-liquid separation after washing with a washing liquid containing 3.5 mass % to 15 mass % of the aromatic solvent and 85 mass % to 96.5 mass % of the polar solvent. 4. The method for producing polyphenylene ether of claim 1 , wherein the washing liquid contains 3.5 mass % to 15 mass % of the aromatic solvent and 85 mass % to 96.5 mass % of the polar solvent. 5. The method for producing polyphenylene ether of claim 1 , wherein polyphenylene ether is obtained in which content of polyphenylene ether components having a molecular weight of 500 or less is 0.3 mass % or less. 6. The method for producing polyphenylene ether of claim 1 , further comprising obtaining a recovered solution or a purified recovered solution resulting from purification of the recovered solution, the recovered solution containing at least one selected from the group consisting of a separated liquid separated in the solid-liquid separating, a separated liquid separated in the washing and solid-liquid separation process, and a condensate liquefied from vent gas vaporized in the drying, wherein the recovered solution or the purified recovered solution that is obtained is used as the washing liquid. 7. The method for producing polyphenylene ether of claim 3 , further comprising obtaining a recovered solution or a purified recovered solution resulting from purification of the recovered solution, the recovered solution containing at least one selected from the group consisting of a separated liquid separated in the solid-liquid separating, a separated liquid separated in the washing and solid-liquid separation process, and a condensate liquefied from vent gas vaporized in the drying, wherein the recovered solution or the purified recovered solution that is obtained is used as the washing liquid. 8. The method for producing polyphenylene ether of claim 4 , further comprising obtaining a recovered solution or a purified recovered solution resulting from purification of the recovered solution, the recovered solution containing at least one selected from the group consisting of a separated liquid separated in the solid-liquid separating, a separated liquid separated in the washing and solid-liquid separation process, and a condensate liquefied from vent gas vaporized in the drying, wherein the recovered solution or the purified recovered solution that is obtained is used as the washing liquid.
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