Production method for polyphenylene ether powder

A manufacturing method and polyphenylene ether technology are applied in the manufacturing field of polyphenylene ether powder, which can solve the problems of insufficient stability, high residual solvent content, difficult liquid additives, etc., achieve excellent solvent solubility, reduce solvent consumption, The effect of less residual solvent

Inactive Publication Date: 2013-12-04
ASAHI KASEI KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In the above-mentioned conventional production method of PPE, there are following problems: the particle size of the precipitated PPE particles is large, resulting in poor dryness and a large amount of residual solvent.
Moreover, the PPE powder produced by the above-mentioned existing PPE production method also has the problem of poor solvent solubility and difficulty in blending with liquid additives
In addition, when the PPE powder produced by the above-mentioned conventional PPE production method is made into a composite and processed into a modified PPE resin, there is a problem that the residual solvent volatilizes and the Residual solvent gas in the extruder etc. flows back, resulting in poor material seizure, or the above-mentioned volatilized solvent gas causes deterioration of the working environment, etc.
[0013] In addition, in the above-mentioned existing PPE manufacturing method, in the precipitation process of PPE, the precipitation is carried out in the region where the concentration of PPE is low, so a large amount of solvent is required, and the efficiency is low. Especially when the solvent is recycled and used, it is also has the problem of very large recycling costs
[0014] Patent Document 1 discloses a technology in which a reciprocating mixer is used to obtain PPE with less scattering of fine powder in the subsequent process and less seizure of the extruder. However, there is a problem that the precipitation process runs When the stability is insufficient, the particle size changes periodically, resulting in large particles and fine powder
[0015] In addition, Patent Document 2 discloses a technique in which PPE particles with a uniform particle size are precipitated using a draft tube-type precipitation device, but this technique is a precipitation technique in a region where the polymer concentration is low, and has Problems with very high solvent usage and low efficiency
[0016] In addition, there is also a problem that the strength of the PPE particles obtained by this technique is insufficient, and micronization occurs in the post-treatment process (for example, a slurry pump, a solid-liquid separator, etc.) after the precipitation process of the PPE particles, and the particles Radius distribution widens
[0018] However, the technique described in Patent Document 3 also has problems in that the precipitation is unstable and the efficiency is low, including precipitation in a region where the polymer concentration is low.

Method used

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  • Production method for polyphenylene ether powder
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Examples

Experimental program
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Effect test

Embodiment

[0261] Hereinafter, the present invention will be specifically described by giving specific examples and comparative examples for comparison therewith, but the present invention is not limited to the following examples.

[0262] First, measurement methods of physical properties and characteristics applied to Examples and Comparative Examples are shown below.

[0263] ((1) Measurement of average particle size and fine powder ratio)

[0264] The PPE powders obtained in Examples and Comparative Examples described later were sieved using a micro-electromagnetic vibrating sieve (M-2 type manufactured by Tsutsui Rika Instruments Co., Ltd.), and the mass of each classifier was measured.

[0265] From the cumulative curve of the particle size distribution, the diameter (median diameter) of the particles corresponding to the central cumulative value was defined as the average particle diameter.

[0266] Similarly, the content (mass %) of the obtained particles of 5.02 μm or less was c...

manufacture example 1

[0300] In a 40-liter jacketed polymerization tank (the bottom of the polymerization tank is equipped with a nozzle for introducing oxygen-containing gas, a turbine impeller and a baffle, and the exhaust line on the upper part of the polymerization tank is equipped with a reflux condenser), one side is filled with 0.5 L Nitrogen gas was blown in at a flow rate of 4.57 g, 24.18 g of 47 mass % hydrogen bromide aqueous solution, 11.00 g of di-tert-butylethylenediamine, 62.72 g of di-n-butylamine, 149.92 g of butyl Dimethylamine, 20.65 kg of toluene, and 3.12 kg of 2,6-dimethylphenol were stirred until a uniform solution was formed and the inner temperature of the polymerization tank was 25°C.

[0301] Next, dry air was introduced from the nozzle into the polymerization tank at a rate of 32.8 NL / min to start polymerization. Dry air was blown for 185 minutes to obtain a polymerization mixture. In addition, during polymerization, internal temperature was controlled to 40 degreeC. T...

manufacture example 2

[0305] The molecular weight was controlled by changing the polymerization time by setting the drying air supply time to 125 minutes. Other conditions were the same as in Production Example 1 to obtain a polymer solution. The obtained polymer solution was referred to as polymer solution (2).

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Abstract

The invention provides a production method for polyphenylene ether (PPE) powder. The method can stably produce PPE powder with uniform small particle size, small residual solvent amount, excellent solvent solubility and easy blend with a liquid additive. The production method for the PPE powder comprises a polymerization step of polymerizing a phenolic compound in a good solvent of PPE to obtain a polymer solution and a precipitation step for generating a slurry by adding the polymer solution and a poor solvent relative to PPE in a precipitation tank and precipitating PPE. In the polymer solution added in the precipitation tank, when a concentration of PPE in a good solvent is set as X (mass%) and a mass ratio (poor solvent/good solvent) of the poor solvent added in the precipitation tank to the good solvent in the polymer solution is set as Y, X and Y meet the following formulas (I) and (II): 30<X<=48...(I); 18.032*(X/100)<2>-1.1873*(X/100)-0.3463<=Y<=22.430*(X/100)<2>-1.4769*(X/100)-0.1868 (II).

Description

technical field [0001] The invention relates to a method for producing polyphenylene ether powder. Background technique [0002] For a long time, the modified PPE resin made of polyphenylene ether (hereinafter sometimes simply referred to as "PPE") as a raw material can produce products and parts of desired shape through melt injection molding, melt extrusion molding and other molding methods. , Therefore, it is widely used as a material for products and components in the electrical and electronic fields, automobile fields, and other various industrial material fields. [0003] In recent years, as new industrial applications of PPE, applications as composite materials for combining with other resins to obtain excellent properties, applications for coating surfaces, and the like are being studied. In particular, dissolving PPE in an aromatic organic solvent such as benzene or toluene, and coating or coating by coating on the surface of inorganic substances such as metal, gla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/46C08G65/38
Inventor 山本繁近藤知宏三井昭
Owner ASAHI KASEI KK
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