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Process for preparing polyphenylene oxide

A polyphenylene ether and phenol compound technology, applied in the field of polyphenylene ether preparation, can solve problems such as inability to suppress foaming, no recovery efficiency, and productivity requirements

Inactive Publication Date: 2008-10-01
ASAHI KASEI KK +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, even if a so-called effective antifoaming agent is used for distilling general aromatic organic solvents, for example, even if a silicone-based antifoaming agent is used, when the good solvent phase is distilled during the production of polyphenylene ether, it cannot suppress foaming in the distillation column. Bubbles, good solvents can only be recovered under distillation conditions that take into account the bubbles
[0007] In the related industries that need to recover high-purity good solvents for the preparation of polyphenylene ether, there is no technology that fully meets the requirements of recovery efficiency and productivity

Method used

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  • Process for preparing polyphenylene oxide
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  • Process for preparing polyphenylene oxide

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preparation example Construction

[0038] The method for preparing polyphenylene ether of the present invention is to add at least one poor solvent of polyphenylene ether selected from methanol, ethanol, isopropanol, n-butanol, acetone and methyl ethyl ketone to the polyphenylene ether solution to precipitate A method for producing polyphenylene ether by filtering polyphenylene ether particles, characterized in that, when recovering a good solvent by distilling a mixture of filtered polyphenylene ether particles, one or more kinds of antifoaming agents selected from fluorosilicone compounds are used. defoamer.

[0039] In the method for producing polyphenylene ether according to the present invention, when recovering the good solvent, it is preferable to add 0.01 to 10 ppm of one or more antifoaming agents selected from fluorosilicone compound-based antifoaming agents with respect to 1 part by weight of the good solvent, more preferably Preferably it is 0.03-7 ppm, particularly preferably 0.05-5 ppm.

[0040] ...

Embodiment 1

[0056] When distillation is performed using a 45 mmφ Oldershaw type fractionation device made of glass with 40 concentration stages as shown in FIG. The solvent phase was distilled.

[0057] 5 kg of toluene was placed in the liquid storage tank of the lowest stage of the Oldershaw type fractionation apparatus, and the liquid storage tank was heated by an oil bath set at 160°C.

[0058] After toluene was distilled off from the uppermost part of the fractionating device, it was cooled and returned to the uppermost stage.

[0059] After confirming that the temperature of the gas phase in the uppermost stage is stable to 110°C, supply the good solvent phase with the aforementioned defoamer added at a rate of 2700 g / hour from the position of the upper 20 stages of the fractionating device, and cool the liquid obtained from the gas phase in the uppermost stage Withdraw 10% and return 90% to the uppermost stage.

[0060] The lowermost gas phase is cooled and extracted.

[0061] Fi...

Embodiment 2

[0079] As in Example 1, foaming was evaluated using the distillation evaluation apparatus shown in FIG. .

[0080] The above-mentioned good solvent phase 300ml that has added defoamer is packed in the 2L cylindrical glass container that has the nitrogen conduit that has spherical filter at the top and distillation pipe, cooling pipe, thermometer as shown in Figure 2, and this container is set in an oil bath set at 100 °C.

[0081] Nitrogen gas was blown in at 20 L / min through the nitrogen gas conduit.

[0082] Thirty minutes after the start of nitrogen blowing, the foaming height of the liquid was observed.

[0083] During this period, the maximum blister height was 8mm.

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Abstract

A method used for preparing polyphenylene oxide comprises steps of introducing oxygen-containing gas to a polymerization solution formed by a good solvent of polyphenylene oxide, a metal salt, an amine compound as well as a phenol compound to oxidate said phenol compound for an oxidative polymerization, mixing a chelating agent aqueous solution into the polymerization solution to stop polymerizaton reaction, adding a poor solvent of polyphenylene oxide into the polyphenylene oxide solution which is obtained by separating the metal salet, the chelating agent and water to precipitate polyphenylene oxide grains, and then filtering said polyphenylene oxide grains to get a polyphenylene oxide product. Said method is characterized in that one or more defoaming agents selected from the fluorosilicone compound type defoaming agents are used when one one recovers the good solvent by distillating the mixing solution obtained by filtering the polyphenylene oxide grains.

Description

technical field [0001] The invention relates to a method for preparing polyphenylene ether. In a polymerization solution composed of a good solvent, a metal salt, an amine compound and a phenol compound, an oxygen-containing gas is passed through to oxidize and polymerize the phenol compound to obtain polyphenylene ether. The polymerization is stopped by mixing the chelating agent aqueous solution, and the poor solvent of polyphenylene ether is added to the polyphenylene ether solution obtained by separating the metal salt, the chelating agent, and water to precipitate polyphenylene ether particles, and the good solvent can be recovered effectively. Background technique [0002] The polyphenylene ether resin composition using polyphenylene ether as a raw material can be used to produce products and parts of the desired shape by molding methods such as melt injection molding or melt extrusion molding. Plastic materials that are widely used as materials for products and compon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/38C08G65/46C08G65/44
Inventor 山本繁前田睦山崎达也武田祐二
Owner ASAHI KASEI KK
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