JPH0812875A - Production of polyphenylene oxide-based molding material - Google Patents
Production of polyphenylene oxide-based molding materialInfo
- Publication number
- JPH0812875A JPH0812875A JP14736994A JP14736994A JPH0812875A JP H0812875 A JPH0812875 A JP H0812875A JP 14736994 A JP14736994 A JP 14736994A JP 14736994 A JP14736994 A JP 14736994A JP H0812875 A JPH0812875 A JP H0812875A
- Authority
- JP
- Japan
- Prior art keywords
- polyphenylene oxide
- molding material
- ppo
- diallyl
- producing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、例えば電子部品等の成
形品を製造するのに使用されるポリフェニレンオキサイ
ド系成形材料の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a polyphenylene oxide-based molding material used for producing molded articles such as electronic parts.
【０００２】[0002]
【従来の技術】通信機器等に使用される一部の電子部品
では、電子部品を構成する成形品に対し、高周波領域で
の誘電正接が低いという高周波特性が要求される。そし
て、このような高周波特性を有する樹脂としてポリフェ
ニレンオキサイドが知られている。しかし、ポリフェニ
レンオキサイドは高融点であり、単独では成形が困難で
あるという問題と耐薬品性が劣るという問題があった。
そこで、実用的な成形温度での成形を可能にし、かつ、
耐薬品性等の性能を改善する方法として、ポリフェニレ
ンオキサイドと架橋剤と開始剤を含む樹脂組成物が提案
されている。（特開昭６３−２６４６６２、特開平３−
２６５６５２等）しかし、ポリフェニレンオキサイドの
融点が高いためにポリフェニレンオキサイドと架橋剤と
を単なる乾式混合で均一に混合することは困難であり、
そのため、単なる乾式混合では成形品の耐薬品性等の性
能改善効果が不十分であった。2. Description of the Related Art Some electronic components used in communication equipment are required to have high frequency characteristics such that a dielectric loss tangent in a high frequency region is low for a molded product forming the electronic component. Polyphenylene oxide is known as a resin having such high frequency characteristics. However, since polyphenylene oxide has a high melting point, it has a problem that molding alone is difficult and a problem that chemical resistance is poor.
Therefore, it enables molding at a practical molding temperature, and
As a method for improving performance such as chemical resistance, a resin composition containing polyphenylene oxide, a cross-linking agent and an initiator has been proposed. (JP-A-63-264662, JP-A-3-
However, since the melting point of polyphenylene oxide is high, it is difficult to uniformly mix polyphenylene oxide and a crosslinking agent by simple dry mixing.
Therefore, the effect of improving the performance such as the chemical resistance of the molded product is not sufficient by simple dry mixing.
【０００３】また、ポリフェニレンオキサイドと架橋剤
とを均一に混合する方法として、トリクロロエチレン、
クロロホルム等のハロゲン化炭化水素等の溶媒に溶解
し、次いで溶媒を除去して樹脂組成物（成形材料等）を
得る方法が知られているが、溶媒を除去するためには多
くのエネルギーを要し、また、ハロゲン化炭化水素等の
溶媒を使用することは環境問題の点で問題があり、他の
方法への転換が求められるようになってきている。As a method for uniformly mixing polyphenylene oxide and a crosslinking agent, trichloroethylene,
A method of obtaining a resin composition (molding material, etc.) by dissolving in a solvent such as halogenated hydrocarbon such as chloroform and then removing the solvent is known, but a large amount of energy is required to remove the solvent. However, the use of a solvent such as a halogenated hydrocarbon is problematic in terms of environmental problems, and conversion to another method has been required.
【０００４】[0004]
【発明が解決しようとする課題】上記の事情に鑑み、本
発明が解決しようとする課題は、ハロゲン化炭化水素等
の溶媒を使用することなしに、耐薬品性に優れる成形品
が得られる、ポリフェニレンオキサイドと架橋剤と開始
剤を含む成形材料の製造方法を開発することである。す
なわち、本発明の目的は、実用的な成形温度で成形が可
能であり、耐薬品性の優れる成形品が得られるポリフェ
ニレンオキサイド系成形材料の製造方法であって、か
つ、ハロゲン化炭化水素等の溶媒を使用していない製造
方法を提供することである。In view of the above circumstances, the problem to be solved by the present invention is to obtain a molded article excellent in chemical resistance without using a solvent such as a halogenated hydrocarbon. The purpose is to develop a method for producing a molding material containing polyphenylene oxide, a cross-linking agent, and an initiator. That is, an object of the present invention is a method for producing a polyphenylene oxide-based molding material that can be molded at a practical molding temperature and that can provide a molded article having excellent chemical resistance, and a halogenated hydrocarbon or the like. It is to provide a manufacturing method which does not use a solvent.
【０００５】[0005]
【課題を解決するための手段】本発明の請求項１に係る
ポリフェニレンオキサイド系成形材料の製造方法は、ポ
リフェニレンオキサイド、ジアリルフタレート類及びパ
ーオキサイドを含有し、ポリフェニレンオキサイドとジ
アリルフタレート類の合計量に対するポリフェニレンオ
キサイドの含有割合が１０〜８０重量％であるポリフェ
ニレンオキサイド系成形材料の製造方法であって、ポリ
フェニレンオキサイドとジアリルフタレート類の混合物
をポリフェニレンオキサイドとジアリルフタレート類の
１相領域において相溶化させることを特徴としている。A method for producing a polyphenylene oxide-based molding material according to claim 1 of the present invention contains polyphenylene oxide, diallyl phthalates and peroxides, and is based on the total amount of polyphenylene oxide and diallyl phthalates. A method for producing a polyphenylene oxide-based molding material having a polyphenylene oxide content of 10 to 80% by weight, comprising compatibilizing a mixture of polyphenylene oxide and diallyl phthalates in a one-phase region of polyphenylene oxide and diallyl phthalates. It has a feature.
【０００６】本発明の請求項２に係るポリフェニレンオ
キサイド系成形材料の製造方法は、請求項１記載のポリ
フェニレンオキサイド系成形材料の製造方法において、
ジアリルフタレート類がジアリルフタレート及び／また
はジアリルイソフタレートであることを特徴としてい
る。A method for producing a polyphenylene oxide-based molding material according to claim 2 of the present invention is the same as the method for producing a polyphenylene oxide-based molding material according to claim 1.
It is characterized in that the diallyl phthalates are diallyl phthalate and / or diallyl isophthalate.
【０００７】本発明の請求項３に係るポリフェニレンオ
キサイド系成形材料の製造方法は、請求項１または請求
項２記載のポリフェニレンオキサイド系成形材料の製造
方法において、ポリフェニレンオキサイドの平均粒子径
が５００μｍ以下であることを特徴としている。The method for producing a polyphenylene oxide-based molding material according to claim 3 of the present invention is the same as the method for producing a polyphenylene oxide-based molding material according to claim 1 or 2, wherein the average particle diameter of the polyphenylene oxide is 500 μm or less. It is characterized by being.
【０００８】本発明の請求項４に係るポリフェニレンオ
キサイド系成形材料の製造方法は、請求項１、請求項２
または請求項３記載のポリフェニレンオキサイド系成形
材料の製造方法において、パーオキサイドの含有量がジ
アリルフタレート類１００重量部に対し０．５〜６重量
部であることを特徴としている。The method for producing a polyphenylene oxide-based molding material according to claim 4 of the present invention is the method according to claim 1 or claim 2.
Alternatively, in the method for producing a polyphenylene oxide-based molding material according to claim 3, the content of peroxide is 0.5 to 6 parts by weight with respect to 100 parts by weight of diallyl phthalate.
【０００９】以下、本発明を詳細に説明する。本発明で
使用されるポリフェニレンオキサイド（以下ＰＰＯと記
す）は一般式が下記式で表される。なお、式中のＲ
は炭素数１〜３の炭化水素基を表し、各Ｒは同じであっ
てもよく、異なってもよい。また、式中のｎは繰り返
し単位を示す正数である。The present invention will be described in detail below. The polyphenylene oxide (hereinafter referred to as PPO) used in the present invention has a general formula represented by the following formula. Note that R in the formula
Represents a hydrocarbon group having 1 to 3 carbon atoms, and each R may be the same or different. Further, n in the formula is a positive number indicating a repeating unit.
【００１０】[0010]
【化１】 Embedded image
【００１１】上記式で表されるＰＰＯの一例として
は、ポリ（２，６−ジメチル−１，４−フェニレンオキ
サイド）があげられる。このようなＰＰＯは、例えば、
ＵＳＰ４０５９５６８号明細書に開示されている方法で
合成することができる。An example of PPO represented by the above formula is poly (2,6-dimethyl-1,4-phenylene oxide). Such PPO is, for example,
It can be synthesized by the method disclosed in USP 4059568.
【００１２】本発明で使用するジアリルフタレート類と
しては、具体的にはジアリルフタレート（以下ＤＡＰと
記す）やジアリルイソフタレート（以下ＤＡＩＰと記
す）があげられるが、それらのプレポリマーであっても
よい。Specific examples of the diallyl phthalates used in the present invention include diallyl phthalate (hereinafter referred to as DAP) and diallyl isophthalate (hereinafter referred to as DAIP), and their prepolymers may also be used. .
【００１３】本発明では、ＰＰＯとジアリルフタレート
類の合計量に対するＰＰＯの含有割合は１０〜８０重量
％に限定される。この理由は、ＰＰＯの含有割合が１０
重量％未満では非常にもろい成形品となり、成形品とし
ての形状保持が困難であるという問題があり、また、Ｐ
ＰＯの含有割合が８０重量％を越えると成形品の耐薬品
性が不十分となるという問題が生じるためである。In the present invention, the content ratio of PPO to the total amount of PPO and diallyl phthalates is limited to 10 to 80% by weight. The reason is that the content ratio of PPO is 10
If it is less than 10% by weight, the resulting product will be very brittle, and it will be difficult to maintain the shape of the product.
This is because if the PO content exceeds 80% by weight, the chemical resistance of the molded product becomes insufficient.
【００１４】本発明は、ＰＰＯとジアリルフタレート類
の混合物をＰＰＯとジアリルフタレート類の１相領域に
おいて相溶化させる点に特徴がある。すなわち、本発明
者等はＰＰＯとジアリルフタレート類の混合物には相溶
化する１相領域が存在し、この１相領域で相溶化させる
と、溶媒を使用しない方法でも、優れた耐薬品性を有す
る成形品が得られることを見出し、本発明に到ったもの
である。従来、ＰＰＯとジアリルフタレート類系の相図
は未解明であり、知見がなかったが、この点を検討した
ところ、互いに相溶化する１相領域が存在することを確
認できた。The present invention is characterized in that a mixture of PPO and diallyl phthalates is compatibilized in the one-phase region of PPO and diallyl phthalate. That is, the present inventors have a one-phase region that compatibilizes in a mixture of PPO and diallyl phthalate, and when the compatibilization is performed in this one-phase region, excellent chemical resistance is obtained even in a method that does not use a solvent. The inventors have found that a molded product can be obtained and have reached the present invention. Conventionally, the phase diagrams of PPO and diallyl phthalates have not been elucidated and no findings have been found. However, when this point was examined, it was confirmed that there was a one-phase region compatibilized with each other.
【００１５】本発明では、短時間でＰＰＯとジアリルフ
タレート類の混合物を相溶化させるには、ＰＰＯの平均
粒子径が５００μｍ以下であることが好ましく、また、
ＰＰＯの最大粒子径は１．０ｍｍ以下であることが好ま
しい。ＰＰＯの平均粒子径が５００μｍを越える場合に
は、相溶化させるのに長時間を要するため、空気雰囲気
中で相溶化させた場合には、樹脂の変色という問題を生
じる場合がある。In the present invention, in order to compatibilize the mixture of PPO and diallyl phthalates in a short time, the average particle diameter of PPO is preferably 500 μm or less.
The maximum particle size of PPO is preferably 1.0 mm or less. When the average particle size of PPO exceeds 500 μm, it takes a long time to make the compatibilize. Therefore, when the PPO is made to compatibilize in an air atmosphere, a problem of discoloration of the resin may occur.
【００１６】本発明で使用するパーオキサイドは架橋剤
であるジアリルフタレート類の反応を開始させるための
開始剤であって、従来より使用されている任意のものが
使用できるが、高温時に蒸発しにくく、添加する温度に
おいて半減時間が１時間以上、特に５時間以上のものが
好ましい。パーオキサイドとしてはα，α’−ビス（ｔ
−ブチル−オキシ−ｍ−イソプロピル）ベンゼン（以下
ＰＢＰと記す）、ジ−ｔ−ブチルパーオキサイド（以下
ＰＢＤと記す）や過酸化ベンゾイル（以下ＢＰＯと記
す）等が例示できる。The peroxide used in the present invention is an initiator for initiating the reaction of a diallyl phthalate which is a cross-linking agent, and any conventionally used one can be used, but it is difficult to evaporate at a high temperature. It is preferable that the half-life at the temperature of addition is 1 hour or longer, particularly 5 hours or longer. As a peroxide, α, α′-bis (t
Examples thereof include -butyl-oxy-m-isopropyl) benzene (hereinafter referred to as PBP), di-t-butyl peroxide (hereinafter referred to as PBD), benzoyl peroxide (hereinafter referred to as BPO), and the like.
【００１７】本発明におけるパーオキサイドの添加量は
ジアリルフタレート類１００重量部に対し０．５〜６重
量部であることが望ましい。０．５重量部未満であると
成形品の耐薬品性に悪影響を及ぼし、６重量部を越える
と成形品が酸化されるためと推定されるが樹脂の変色が
生じやすくなり、それに伴って、成形品の誘電率も高く
なるという問題が生じる。また、本発明におけるパーオ
キサイドの添加のタイミングは、特に限定するものでは
ないが、ＰＰＯとジアリルフタレート類の混合物を相溶
化させた後、ＰＰＯとジアリルフタレート類の１相領域
内のできるだけ低温度域で添加することが好ましい。The amount of peroxide added in the present invention is preferably 0.5 to 6 parts by weight based on 100 parts by weight of diallyl phthalates. If it is less than 0.5 parts by weight, the chemical resistance of the molded product is adversely affected, and if it exceeds 6 parts by weight, it is presumed that the molded product is oxidized, but discoloration of the resin is likely to occur. There is a problem that the dielectric constant of the molded product also becomes high. The timing of addition of peroxide in the present invention is not particularly limited, but after the mixture of PPO and diallyl phthalate is compatibilized, the temperature is as low as possible within one phase region of PPO and diallyl phthalate. Is preferably added.
【００１８】また、本発明では、本発明の目的を損なわ
ない範囲で他の成分を含有させることができる。特に、
ポリスチレンをＰＰＯと共に使用すると、相溶域が広が
るので、より低温で相溶化させることが可能になり好ま
しい。ただし、ポリスチレンの添加量を増すと共に耐薬
品性が損なわれるので、ポリスチレンの添加量はＰＰ
Ｏ、ジアリルフタレート類及びポリスチレンの合計量の
３０重量％以下までとするのが好ましい。Further, in the present invention, other components may be contained within the range not impairing the object of the present invention. In particular,
When polystyrene is used together with PPO, the compatible region is widened, so that it is possible to achieve compatibilization at a lower temperature, which is preferable. However, since the chemical resistance is impaired as the amount of polystyrene added increases, the amount of polystyrene added is PP.
It is preferably up to 30% by weight of the total amount of O, diallyl phthalates and polystyrene.
【００１９】[0019]
【作用】ＰＰＯとジアリルフタレート類の混合物をＰＰ
Ｏとジアリルフタレート類の１相領域において相溶化さ
せることは、ハロゲン化炭化水素等の溶媒を使用するこ
となしに、混合物を均一に混合する働きをする。[Function] A mixture of PPO and diallyl phthalates is added to PP.
Compatibilizing O and diallyl phthalates in the one-phase region serves to uniformly mix the mixture without the use of solvents such as halogenated hydrocarbons.
【００２０】また、ＰＰＯの平均粒子径が５００μｍ以
下であることは、相溶化させるための時間を短縮する働
きをする。When the average particle size of PPO is 500 μm or less, it serves to shorten the time for compatibilization.
【００２１】また、パーオキサイドの含有量がジアリル
フタレート類１００重量部に対し０．５〜６重量部であ
ることは、ジアリルフタレート類の反応を適切に行なえ
るようにする働きをする。When the content of the peroxide is 0.5 to 6 parts by weight with respect to 100 parts by weight of the diallyl phthalates, the function of allowing the reaction of the diallyl phthalates to be carried out appropriately.
【００２２】[0022]
【実施例】以下、本発明を実施例及び比較例に基づいて
説明する。なお、各実施例及び各比較例では、ＰＰＯと
して日本ＧＥプラスチック社製の、Ｍw ／Ｍn ＝４．２
であり、Ｍw が約５０，０００のものを使用した。 （実施例１）表１に示す配合割合で、ＰＰＯ（平均粒子
径１００μｍのもの）とＤＡＰを配合したものを、攪拌
しながら、１４５℃で３０分間保持した。（この温度を
攪拌温度として表１に示す。）ＰＰＯとＤＡＰが相溶化
して透明になったのを確認した後、冷却し、表１に示す
パーオキサイドの添加温度である１４０℃になったとき
に、パーオキサイドとしてＰＢＰをＤＡＰ１００重量部
に対して２．０重量部の割合で添加し、２分間攪拌し
た。次いで室温まで冷却して成形材料を得た。得られた
成形材料について、均一性を外観の透明性で評価し、透
明性が良好であれば○、透明性がなければ×として表１
にその結果を示した。また、得られた成形材料を用い
て、１８０℃、１０分間金型内で成形して硬化させ、次
いでオーブンで１８０℃、２時間加熱して１０ｍｍ×５
０ｍｍ×２ｍｍの平板状の成形品を得た。得られた成形
品をトリクロロエチレン中に、室温で７０時間浸漬し、
溶剤による抽出量を求めて、耐薬品性を評価した。この
結果を表１に示した。EXAMPLES The present invention will be described below based on Examples and Comparative Examples. In each of the examples and the comparative examples, Pw manufactured by Japan GE Plastics Co., Ltd., M w / M n = 4.2.
And M w of about 50,000 was used. Example 1 A mixture of PPO (having an average particle size of 100 μm) and DAP in the mixing ratio shown in Table 1 was kept at 145 ° C. for 30 minutes while stirring. (This temperature is shown as a stirring temperature in Table 1.) After confirming that PPO and DAP were compatibilized and became transparent, the mixture was cooled to 140 ° C., which is the addition temperature of peroxide shown in Table 1. At this time, PBP as a peroxide was added at a ratio of 2.0 parts by weight to 100 parts by weight of DAP, and the mixture was stirred for 2 minutes. Then, it was cooled to room temperature to obtain a molding material. With respect to the obtained molding material, the uniformity was evaluated by the transparency of the appearance, and when the transparency was good, the result was ◯, and when there was no transparency, the result was x.
The results are shown in. Further, using the obtained molding material, it is molded and cured in a mold at 180 ° C. for 10 minutes, and then heated in an oven at 180 ° C. for 2 hours to obtain 10 mm × 5.
A 0 mm × 2 mm flat plate-shaped molded product was obtained. The resulting molded product is immersed in trichlorethylene at room temperature for 70 hours,
The chemical resistance was evaluated by determining the amount of solvent extracted. The results are shown in Table 1.
【００２３】（実施例２〜５）ＰＰＯ（平均粒子径１０
０μｍのもの）とＤＡＰの配合割合、攪拌温度、パーオ
キサイドの添加温度を表１に示す条件にした以外は、実
施例１と同様にして成形材料及び平板状の成形品を得
た。得られた成形材料及び平板状の成形品について、実
施例１と同様の評価を行い、その結果を表１に示した。
なお、実施例２〜５では攪拌温度で３０分間保持した後
の状態は透明であり、ＰＰＯとＤＡＰが相溶化している
ことが確認された。(Examples 2 to 5) PPO (average particle size 10
0 μm) and DAP, the mixing temperature, the stirring temperature, and the peroxide addition temperature were set to the conditions shown in Table 1 in the same manner as in Example 1 to obtain a molding material and a flat-plate molded article. The obtained molding material and flat plate-shaped molded product were evaluated in the same manner as in Example 1, and the results are shown in Table 1.
In addition, in Examples 2 to 5, the state after being kept at the stirring temperature for 30 minutes was transparent, and it was confirmed that PPO and DAP were compatibilized.
【００２４】（比較例１〜３）ＰＰＯ（平均粒子径１０
０μｍのもの）とＤＡＰの配合割合、攪拌温度、パーオ
キサイドの添加温度を表２に示す条件にした以外は、実
施例１と同様にして成形材料及び平板状の成形品を得
た。得られた成形材料及び平板状の成形品について、実
施例１と同様の評価を行い、その結果を表２に示した。
なお、比較例１及び比較例２では攪拌温度で３０分間保
持した後の状態は不透明であり、相溶化物は得られなか
った。このことは、比較例１及び比較例２の配合割合と
攪拌温度の組合せはＰＰＯとＤＡＰの混合物の１相領域
外であったことを示している。また、比較例３ではＰＰ
Ｏの原料をそのまま成形材料として用いたため、１８０
℃、１０分間の金型内の成形では溶融せず成形品は得ら
れなかった。この、金型内での加熱終了後、得られたも
のをオーブンで１８０℃、２時間加熱し、次いで得られ
たＰＰＯ単独物の耐薬品性を評価した。この結果を表２
に示した。Comparative Examples 1 to 3 PPO (average particle size 10
0 μm) and DAP, the stirring temperature, and the addition temperature of peroxide were set to the conditions shown in Table 2 in the same manner as in Example 1 to obtain a molding material and a flat molded article. The obtained molding material and flat plate-shaped molded product were evaluated in the same manner as in Example 1, and the results are shown in Table 2.
In Comparative Examples 1 and 2, the state after being kept at the stirring temperature for 30 minutes was opaque, and a compatibilized product was not obtained. This indicates that the combination of the mixing ratio and the stirring temperature in Comparative Examples 1 and 2 was outside the one-phase region of the mixture of PPO and DAP. In Comparative Example 3, PP
Since the raw material of O was used as it was as the molding material,
Molding in a mold at 10 ° C. for 10 minutes did not melt and a molded product could not be obtained. After completion of the heating in the mold, the obtained product was heated in an oven at 180 ° C. for 2 hours, and then the chemical resistance of the obtained PPO alone was evaluated. The results are shown in Table 2.
It was shown to.
【００２５】[0025]
【表１】 [Table 1]
【００２６】[0026]
【表２】 [Table 2]
【００２７】（実施例６〜１１）表３に示す配合割合
で、ＰＰＯ（平均粒子径は表２に示す）とＤＡＰを配合
したものを、表２に示す攪拌温度で保持し、ＰＰＯとＤ
ＡＰが相溶化して透明になるまで攪拌した。この相溶化
するまでの時間を表３に示した。ＰＰＯとＤＡＰが相溶
化して透明になった時点で、パーオキサイドとしてＰＢ
ＰをＤＡＰ１００重量部に対して２．０重量部の割合で
添加し、２分間攪拌した。次いで室温まで冷却して成形
材料を得た。得られた成形材料について、外観を評価
し、表３にその結果を示した。また、得られた成形材料
を用いて、１８０℃、１０分間金型内で成形して硬化さ
せ、次いでオーブンで１８０℃、２時間加熱して１０ｍ
ｍ×５０ｍｍ×２ｍｍの平板状の成形品を得た。得られ
た成形品をトリクロロエチレン中に、室温で７０時間浸
漬し、溶剤による抽出量を求めて、耐薬品性を評価し
た。この結果も表３に示した。Examples 6 to 11 PPO (average particle size shown in Table 2) and DAP were blended at the blending ratios shown in Table 3 and kept at the stirring temperature shown in Table 2 to obtain PPO and D.
The mixture was stirred until the AP became compatible and became transparent. Table 3 shows the time until this compatibilization occurred. When PPO and DAP are compatibilized and become transparent, PB is converted into peroxide as PB.
P was added at a ratio of 2.0 parts by weight to 100 parts by weight of DAP and stirred for 2 minutes. Then, it was cooled to room temperature to obtain a molding material. The appearance of the obtained molding material was evaluated, and the results are shown in Table 3. Also, using the obtained molding material, it is molded and cured in a mold at 180 ° C. for 10 minutes, and then heated in an oven at 180 ° C. for 2 hours to 10 m.
A flat molded product of m × 50 mm × 2 mm was obtained. The obtained molded product was immersed in trichlorethylene at room temperature for 70 hours, and the amount of extraction with a solvent was determined to evaluate the chemical resistance. The results are also shown in Table 3.
【００２８】表３の結果から、短時間でＰＰＯとＤＡＰ
の混合物を相溶化させるには、ＰＰＯの平均粒子径が５
００μｍ以下であることが好ましいことが確認された。
ＰＰＯの平均粒子径が大きくなると、相溶化させるのに
長時間を要し、空気雰囲気中で相溶化させた場合樹脂が
変色するようになることも確認された。From the results of Table 3, PPO and DAP can be obtained in a short time.
In order to compatibilize the mixture of PPO, the average particle size of PPO is 5
It was confirmed that it is preferably 00 μm or less.
It was also confirmed that when the average particle diameter of PPO becomes large, it takes a long time to be compatibilized, and the resin becomes discolored when it is compatibilized in an air atmosphere.
【００２９】[0029]
【表３】 [Table 3]
【００３０】（実施例１２〜１６）表４に示すＰＰＯ
（平均粒子径１００μｍのもの）とＤＡＰの配合割合，
パーオキサイドの種類及びパーオキサイドの添加量とし
た以外は実施例３と同様にして成形材料及び平板状の成
形品を得た。得られた平板状の成形品について、１００
ｋＨｚにおける誘電率、外観及び耐薬品性を評価し、そ
の結果を表４に示した。なお、実施例３で得られた平板
状の成形品についても同様の評価をし、その結果を表４
に示した。(Examples 12 to 16) PPO shown in Table 4
(Average particle size 100 μm) and DAP blending ratio,
A molding material and a flat molded article were obtained in the same manner as in Example 3 except that the type of peroxide and the amount of peroxide added were changed. About the obtained flat plate-shaped molded article, 100
The dielectric constant, appearance and chemical resistance at kHz were evaluated, and the results are shown in Table 4. The flat molded article obtained in Example 3 was also evaluated in the same manner, and the results are shown in Table 4.
It was shown to.
【００３１】表４の結果から、パーオキサイドの添加量
がＤＡＰ１００重量部に対し６重量部を越えると成形品
の変色が生じ、それに伴って、成形品の誘電率も高くな
ることが確認された。From the results shown in Table 4, it was confirmed that when the amount of peroxide added exceeded 6 parts by weight with respect to 100 parts by weight of DAP, discoloration of the molded product occurred, and accordingly the dielectric constant of the molded product also increased. .
【００３２】[0032]
【表４】 [Table 4]
【００３３】（実施例１７〜２１）実施例１７〜２１で
はジアリルフタレート類としてＤＡＩＰを使用した。そ
して、ＰＰＯ（平均粒子径１００μｍのもの）とＤＡＩ
Ｐの配合割合、攪拌温度、パーオキサイドの添加温度を
表５に示す条件にした以外は、実施例１と同様にして成
形材料及び平板状の成形品を得た。得られた成形材料に
ついて均一性（外観の透明性）について評価した。均一
性（外観の透明性）の評価は、前記の実施例１と同様に
して行った。また、得られた平板状の成形品について
も、実施例１と同様の評価を行い、その結果を表５に示
した。なお、実施例１７〜２１は表５に示す攪拌温度で
３０分間保持した後の状態は透明であり、ＰＰＯとＤＡ
ＩＰが相溶化していることが確認された。(Examples 17 to 21) In Examples 17 to 21, DAIP was used as the diallyl phthalates. Then, PPO (with an average particle size of 100 μm) and DAI
A molding material and a flat molded article were obtained in the same manner as in Example 1 except that the mixing ratio of P, the stirring temperature, and the addition temperature of peroxide were set to the conditions shown in Table 5. The obtained molding material was evaluated for uniformity (transparency in appearance). Evaluation of uniformity (transparency of appearance) was performed in the same manner as in Example 1 above. Further, the obtained flat plate-shaped molded product was evaluated in the same manner as in Example 1, and the results are shown in Table 5. In addition, in Examples 17 to 21, the state after being kept at the stirring temperature shown in Table 5 for 30 minutes was transparent, and PPO and DA were used.
It was confirmed that IP was compatibilized.
【００３４】表５の結果から、ＤＡＩＰを用いた場合で
も、実用的な成形温度で成形して、耐薬品性の良好な成
形品が得られることが確認された。From the results shown in Table 5, it was confirmed that even when DAIP was used, a molded article having good chemical resistance could be obtained by molding at a practical molding temperature.
【００３５】[0035]
【表５】 [Table 5]
【００３６】[0036]
【発明の効果】本発明の請求項１及び請求項２に係るＰ
ＰＯ系成形材料の製造方法によれば、ハロゲン化炭化水
素等の溶媒を使用することなしに、ＰＰＯと架橋剤と開
始剤を含む成形材料を製造することができる。そして、
この製造方法によって製造された成形材料によれば、実
用的な成形温度での成形で、耐薬品性の優れる成形品が
得られる。すなわち、この製造方法によれば、環境問題
の点で望ましい方法である、溶媒を除去する工程を必要
としない方法で、優れた性能を有するＰＰＯ系成形材料
を製造できるようになる。EFFECTS OF THE INVENTION P according to claims 1 and 2 of the present invention
According to the method for producing a PO-based molding material, a molding material containing PPO, a cross-linking agent, and an initiator can be manufactured without using a solvent such as a halogenated hydrocarbon. And
According to the molding material manufactured by this manufacturing method, a molded article having excellent chemical resistance can be obtained by molding at a practical molding temperature. That is, according to this manufacturing method, a PPO-based molding material having excellent performance can be manufactured by a method that does not require the step of removing the solvent, which is a desirable method in terms of environmental problems.
【００３７】本発明の請求項３に係るＰＰＯ系成形材料
の製造方法によれば、ＰＰＯの平均粒子径が５００μｍ
以下であることにより、ＰＰＯとジアリルフタレート類
の混合物を相溶化させるための時間を短縮することがで
きる。According to the method for producing a PPO-based molding material according to claim 3 of the present invention, the average particle diameter of PPO is 500 μm.
Due to the following, the time for compatibilizing the mixture of PPO and diallyl phthalates can be shortened.
【００３８】本発明の請求項４に係るＰＰＯ系成形材料
の製造方法によれば、パーオキサイドの含有量がジアリ
ルフタレート類１００重量部に対し０．５〜６重量部で
あることにより、ジアリルフタレート類の反応を適切に
行なえるようにすることができる。According to the method for producing a PPO-based molding material according to the fourth aspect of the present invention, the content of peroxide is 0.5 to 6 parts by weight with respect to 100 parts by weight of diallyl phthalates. The kind of reaction can be properly performed.
Claims (4)
タレート類及びパーオキサイドを含有し、ポリフェニレ
ンオキサイドとジアリルフタレート類の合計量に対する
ポリフェニレンオキサイドの含有割合が１０〜８０重量
％であるポリフェニレンオキサイド系成形材料の製造方
法であって、ポリフェニレンオキサイドとジアリルフタ
レート類の混合物をポリフェニレンオキサイドとジアリ
ルフタレート類の１相領域において相溶化させることを
特徴とするポリフェニレンオキサイド系成形材料の製造
方法。1. A method for producing a polyphenylene oxide-based molding material containing polyphenylene oxide, diallyl phthalates and peroxides, wherein the content of polyphenylene oxide is 10 to 80% by weight based on the total amount of polyphenylene oxide and diallyl phthalates. A method for producing a polyphenylene oxide-based molding material, which comprises compatibilizing a mixture of polyphenylene oxide and diallyl phthalates in a one-phase region of polyphenylene oxide and diallyl phthalates.
ート及び／またはジアリルイソフタレートであることを
特徴とする請求項１記載のポリフェニレンオキサイド系
成形材料の製造方法。2. The method for producing a polyphenylene oxide-based molding material according to claim 1, wherein the diallyl phthalates are diallyl phthalate and / or diallyl isophthalate.
が５００μｍ以下であることを特徴とする請求項１また
は請求項２記載のポリフェニレンオキサイド系成形材料
の製造方法。3. The method for producing a polyphenylene oxide-based molding material according to claim 1, wherein the polyphenylene oxide has an average particle diameter of 500 μm or less.
レート類１００重量部に対し０．５〜６重量部であるこ
とを特徴とする請求項１、請求項２または請求項３記載
のポリフェニレンオキサイド系成形材料の製造方法。4. The polyphenylene oxide molding according to claim 1, wherein the content of peroxide is 0.5 to 6 parts by weight with respect to 100 parts by weight of diallyl phthalates. Material manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14736994A JPH0812875A (en) | 1994-06-29 | 1994-06-29 | Production of polyphenylene oxide-based molding material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14736994A JPH0812875A (en) | 1994-06-29 | 1994-06-29 | Production of polyphenylene oxide-based molding material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0812875A true JPH0812875A (en) | 1996-01-16 |
Family
ID=15428675
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14736994A Pending JPH0812875A (en) | 1994-06-29 | 1994-06-29 | Production of polyphenylene oxide-based molding material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0812875A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6197898B1 (en) | 1997-11-18 | 2001-03-06 | General Electric Company | Melt-mixing thermoplastic and epoxy resin above Tg or Tm of thermoplastic with curing agent |
| WO2002077102A1 (en) * | 2001-03-27 | 2002-10-03 | General Electric Company | Abrasive-filled thermoset composition and its preparation, and abrasive-filled articles and their preparation |
| WO2002077103A1 (en) * | 2001-03-27 | 2002-10-03 | General Electric Company | Poly(arylene ether)-containing thermoset composition in powder form, method for the preparation thereof, and articles derived therefrom |
-
1994
- 1994-06-29 JP JP14736994A patent/JPH0812875A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6197898B1 (en) | 1997-11-18 | 2001-03-06 | General Electric Company | Melt-mixing thermoplastic and epoxy resin above Tg or Tm of thermoplastic with curing agent |
| WO2002077102A1 (en) * | 2001-03-27 | 2002-10-03 | General Electric Company | Abrasive-filled thermoset composition and its preparation, and abrasive-filled articles and their preparation |
| WO2002077103A1 (en) * | 2001-03-27 | 2002-10-03 | General Electric Company | Poly(arylene ether)-containing thermoset composition in powder form, method for the preparation thereof, and articles derived therefrom |
| US6593391B2 (en) | 2001-03-27 | 2003-07-15 | General Electric Company | Abrasive-filled thermoset composition and its preparation, and abrasive-filled articles and their preparation |
| CN100363425C (en) * | 2001-03-27 | 2008-01-23 | 通用电气公司 | Poly (arylene ether)-containing thermoset composition in powder form, method for preparation thereof, and articles derived therefrom |
| KR100823359B1 (en) * | 2001-03-27 | 2008-04-17 | 제너럴 일렉트릭 캄파니 | Abrasive-filled thermoset composition and its preparation, and abrasive-filled articles and their preparation |
| CN100398606C (en) * | 2001-03-27 | 2008-07-02 | 通用电气公司 | Abrasive-filled thermoset composition and its preparation, and abrasive-filled articles and their preparation |
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