JP2000302877A - Preparation of polyphenylene ether powder with improved grain size distribution - Google Patents
Preparation of polyphenylene ether powder with improved grain size distributionInfo
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- JP2000302877A JP2000302877A JP11109658A JP10965899A JP2000302877A JP 2000302877 A JP2000302877 A JP 2000302877A JP 11109658 A JP11109658 A JP 11109658A JP 10965899 A JP10965899 A JP 10965899A JP 2000302877 A JP2000302877 A JP 2000302877A
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- powder
- polyphenylene ether
- fine particles
- particle size
- molded body
- Prior art date
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- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はポリフェニレンエー
テル粉体中の微小粒子を減らすことにより、ポリフェニ
レンエーテル粉体を取り扱い性、安全性に優れ、押し出
し生産性の高い粉体に改良する方法に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for improving polyphenylene ether powder into a powder having excellent handleability, safety and high extrusion productivity by reducing fine particles in the polyphenylene ether powder. is there.
【０００２】[0002]
【従来技術】フェノール性化合物を酸化重合させること
でポリフェニレンエーテルを製造する技術は特公昭４２
−３１９５号公報、特公昭４５−２３５５５号公報、特
開昭６４−３３１３１号公報、特開昭５２−８９７号公
報などに記載されている。これらの方法で重合された重
合体溶液からポリフェニレンエーテル樹脂を回収するに
は、一般にはポリフェニレンエーテルの貧溶媒であるメ
タノール等を加え、重合体を析出することによって回収
する方法が用いられる。この際析出する重合体粒子は著
しく微細な粒子を含んでいる。このため粉体の取り扱い
性が悪く、飛散しやすい性質とともに、粉塵爆発などの
安全性の点でもかなりの配慮が必要であった。また、樹
脂の押し出し造粒時には、粉体特性が悪いため、噛み込
み不良などにより生産性を落とす原因にもなっている。2. Description of the Related Art A technique for producing polyphenylene ether by oxidative polymerization of a phenolic compound is disclosed in Japanese Patent Publication No. Sho 42.
JP-A-31955, JP-B-45-23555, JP-A-64-33131, JP-A-52-897, and the like. In order to recover the polyphenylene ether resin from the polymer solution polymerized by these methods, a method is generally used in which methanol or the like, which is a poor solvent for the polyphenylene ether, is added, and the polymer is recovered by precipitation. The polymer particles precipitated at this time contain extremely fine particles. For this reason, the handling of the powder is poor and the powder is liable to be scattered, and considerable consideration must be given to the safety such as dust explosion. In addition, during extrusion granulation of the resin, the powder characteristics are poor, which causes a drop in productivity due to poor biting or the like.
【０００３】特公昭４５−５８７号公報等に明示されて
いるように、ポリフェニレンエーテル樹脂を含む重合溶
液にポリフェニレンエーテル樹脂の貧溶媒を接触させ、
かかる重合体を析出させる方法においては、重合体を析
出させるときの条件がポリフェニレンエーテル樹脂粒子
径に大きな影響を及ぼすことが既に知られている。この
方法によると重合体溶液をその溶液の沸点近傍まで加熱
し、ポリフェニレンエーテル樹脂の貧溶媒であるメタノ
ール等の添加を、可及的速やかに行わなければならない
ことから操作が困難かつ煩雑であった。As disclosed in Japanese Patent Publication No. 45-587, a poor solvent for a polyphenylene ether resin is brought into contact with a polymerization solution containing the polyphenylene ether resin,
In such a method of precipitating a polymer, it is already known that the conditions at the time of precipitating the polymer have a great effect on the particle diameter of the polyphenylene ether resin. According to this method, the polymer solution is heated to near the boiling point of the solution, and the addition of methanol or the like, which is a poor solvent for the polyphenylene ether resin, must be performed as quickly as possible, which makes the operation difficult and complicated. .
【０００４】また、特公昭５５−１７７７５号公報にお
いては、有機溶媒を含むポリフェニレンエーテル樹脂粉
体の水分散系において熱処理を行うことにより、ポリフ
ェニレンエーテル樹脂粉体の粒子径を肥大化させる方法
が明示されているが、この方法では比熱の高い水を用い
なければならず、エネルギーコストが大きくなってしま
い不利益が多い。Japanese Patent Publication No. 55-17775 discloses a method for enlarging the particle diameter of a polyphenylene ether resin powder by performing a heat treatment in an aqueous dispersion of the polyphenylene ether resin powder containing an organic solvent. However, in this method, water having a high specific heat must be used, which increases the energy cost and disadvantageously.
【０００５】特開平７−９７４４１においては、粉体粒
子の界面活性剤を添加し、粉体に発生する静電気を除去
することによって飛散防止性を改良する試みが述べられ
ている。この方法では、その効果に比べ工程が煩雑であ
り、そのため経済性にも劣るという欠点があった。Japanese Patent Application Laid-Open No. 7-97441 discloses an attempt to improve the anti-scattering property by adding a surfactant of powder particles to remove static electricity generated in the powder. This method has a drawback that the process is complicated as compared with the effect, and therefore the economic efficiency is inferior.
【０００６】[0006]
【発明が解決しようとする課題】ポリフェニレンエーテ
ル粉体の取り扱い性を低下させている原因は、微小粒子
を含んでおり平均粒径が小さいことである。即ち、粉体
取り扱い性の良い粒子とは微小粒子が少なく、適度に粒
度の揃ったものである。従って、ポリフェニレンエーテ
ルの粉体取り扱い性を改善するためには、微小粒子を減
らすことが要求されている。しかし前述のような開示例
では、この目的を達成するためには困難が多い。より簡
便で効率的な方法により、ポリフェニレンエーテル粉体
の取り扱い性を改良することが課題であった。The reason why the handleability of the polyphenylene ether powder is reduced is that it contains fine particles and has a small average particle size. In other words, particles having good powder handling properties are those having few fine particles and moderately uniform particle size. Therefore, in order to improve the powder handling properties of polyphenylene ether, it is required to reduce fine particles. However, in the disclosed examples described above, there are many difficulties in achieving this object. The problem was to improve the handleability of polyphenylene ether powder by a simpler and more efficient method.
【０００７】[0007]
【課題を解決するための手段】本発明者らは上記課題を
解決するため、鋭意検討を進めた結果、驚くべきこと
に、ある特定の温度範囲でポリフェニレンエーテル粉体
に圧力を加えることによって、容易に充分な強度を持つ
成型体が得られることを見出した。更に得られた成型体
を再粉砕すると、微小粒子が大幅に低減された取り扱い
性に優れたポリフェニレンエーテル粉体が得られること
を見出し、本発明に至った。Means for Solving the Problems The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, surprisingly, by applying pressure to polyphenylene ether powder in a specific temperature range, It has been found that a molded product having sufficient strength can be easily obtained. Further, when the obtained molded body is reground, it has been found that a polyphenylene ether powder excellent in handleability, in which fine particles are greatly reduced, is obtained, and the present invention has been achieved.
【０００８】すなわち本発明は、温度５〜２００℃の範
囲のポリフェニレンエーテル粉体を圧縮成型することに
より密度０．７〜１．０５５ｇ／ｃｍ3の成型体を生成
し、得られた成型体を再粉砕することによって粒径１μ
ｍ以下の微小粒子の含有率を全体の０．５重量％以下と
することを特徴とする粒度分布の改良されたポリフェニ
レンエーテル粉体の製造法である。That is, according to the present invention, a molded article having a density of 0.7 to 1.055 g / cm 3 is produced by compression molding a polyphenylene ether powder having a temperature in the range of 5 to 200 ° C. Particle size 1μ by re-milling
A method for producing a polyphenylene ether powder having an improved particle size distribution, wherein the content of fine particles having a particle size of m or less is 0.5% by weight or less based on the whole.
【０００９】以下、発明を詳細に説明する。Hereinafter, the present invention will be described in detail.
【００１０】本発明に用いられるポリフェニレンエーテ
ル樹脂とは、次に示す一般式（１）、The polyphenylene ether resin used in the present invention is represented by the following general formula (1):
【００１１】[0011]
【化１】 Embedded image
【００１２】を繰り返し単位とし、構成単位が上記
［ａ］及び［ｂ］からなる単独重合体、あるいは共重合
体が使用できる。ポリフェニレンエーテル系樹脂の単独
重合体の代表例としては、ポリ（２，６−ジメチル−
１，４フェニレン）エーテル、ポリ（２−メチル−６−
エチル−１，４−フェニレン）エーテル、ポリ（２，６
−ジエチル−１，４−フェニレン）エーテル、ポリ（２
−エチル−６−ｎ−プロピル−１，４−フェニレン）エ
ーテル、ポリ（２，６−ジ−ｎ−プロピル−１，４−フ
ェニレン）エーテル、ポリ（２−メチル−６−ｎ−ブチ
ル−１，４−フェニレン）エーテル、ポリ（２−エチル
−６−イソプロピル−１，４−フェニレン）エーテル、
ポリ（２−メチル−６−クロロエチル−１，４−フェニ
レン）エーテル、ポリ（２−メチル−６−ヒドロキシエ
チル−１，４−フェニレン）エーテル等のホモポリマー
が考えられる。A homopolymer or a copolymer in which the structural units are the above-mentioned [a] and [b] can be used. Representative examples of the homopolymer of the polyphenylene ether resin include poly (2,6-dimethyl-
1,4 phenylene) ether, poly (2-methyl-6-
Ethyl-1,4-phenylene) ether, poly (2,6
-Diethyl-1,4-phenylene) ether, poly (2
-Ethyl-6-n-propyl-1,4-phenylene) ether, poly (2,6-di-n-propyl-1,4-phenylene) ether, poly (2-methyl-6-n-butyl-1) , 4-phenylene) ether, poly (2-ethyl-6-isopropyl-1,4-phenylene) ether,
Homopolymers such as poly (2-methyl-6-chloroethyl-1,4-phenylene) ether and poly (2-methyl-6-hydroxyethyl-1,4-phenylene) ether are conceivable.
【００１３】ポリフェニレンエーテル共重合体は、２，
６ジメチルフェノールと２，３，６−トリメチルフェノ
ールとの共重合体あるいはｏ−クレゾールとの共重合体
あるいは２，３，６−トリメチルフェノール及びｏ−ク
レゾールとの共重合体等、ポリフェニレンエーテル構造
を主体としてなるポリフェニレンエーテル共重合体を包
含する。The polyphenylene ether copolymer is 2,2
A polyphenylene ether structure such as a copolymer of 6-dimethylphenol and 2,3,6-trimethylphenol, a copolymer of o-cresol, or a copolymer of 2,3,6-trimethylphenol and o-cresol It includes a polyphenylene ether copolymer as a main component.
【００１４】また、本発明のポリフェニレンエーテル系
樹脂中には、本発明の主旨に反しない限り、従来ポリフ
ェニレンエーテル樹脂中に存在させてもよいことが提案
されている他の種々のフェニレンエーテルユニットを部
分構造として含んでいても構わない。少量共存させるこ
とが提案されているものの例としては、特開昭６３−１
２６９８号公報及び特開昭６３−３０１２２２号公報に
記載されている、２−（ジアルキルアミノメチル）−６
−メチルフェニレンエーテルユニットや、２−（Ｎ−ア
ルキル−Ｎ−フェニルアミノメチル）−６−メチルフェ
ニレンエーテルユニット等が挙げられる。In the polyphenylene ether-based resin of the present invention, various other phenylene ether units which have been proposed to be allowed to exist in the conventional polyphenylene ether resin without departing from the gist of the present invention are used. It may be included as a partial structure. Japanese Patent Application Laid-Open No. 63-1 / 1988 discloses an example of a proposal for coexistence in a small amount.
2- (dialkylaminomethyl) -6 described in JP-A-2698 and JP-A-63-301222.
-Methylphenylene ether unit and 2- (N-alkyl-N-phenylaminomethyl) -6-methylphenylene ether unit.
【００１５】また、ポリフェニレンエーテル主鎖中にジ
フェノキノン等が少量結合したものも含まれる。[0015] The polyphenylene ether main chain also includes those in which diphenoquinone or the like is bonded in a small amount.
【００１６】更に、例えば特開平２−２７６８２３号公
報、特開昭６３−１０８０５９号公報、特開昭５９−５
９７２４号公報等に記載されている、炭素−炭素二重結
合を持つ化合物より変性されたポリフェニレンエーテル
も含む。Furthermore, for example, JP-A-2-276823, JP-A-63-108059, and JP-A-59-5
Also included are polyphenylene ethers modified from compounds having a carbon-carbon double bond described in JP-A-9724.
【００１７】本発明に用いるポリフェニレンエーテル樹
脂の分子量としては、数平均分子量で１，０００〜１０
０，０００である。その好ましい範囲は、６，０００〜
６０，０００のものである。本発明中の数平均分子量と
は、ゲルパーミエーションクロマトグラフィーにより、
標準ポリスチレンの検量線を用いて求めたポリスチレン
換算の数平均分子量である。The polyphenylene ether resin used in the present invention has a number average molecular weight of 1,000 to 10
It is 0000. The preferred range is 6,000 to
60,000. The number average molecular weight in the present invention, by gel permeation chromatography,
It is a number average molecular weight in terms of polystyrene obtained using a standard polystyrene calibration curve.
【００１８】本発明の方法で得られる粉体の粒径分布に
対する、原料とするポリフェニレンエーテル樹脂の粒径
分布の影響は小さい。そのため原料粉体がより微粒子を
多量に含むものの方が粉体取り扱い性の改良効果が大き
い。原料粉体に含まれる粒径０．５μｍ以下の粒子が全
体の０．００５重量％以上であることが好ましい。更に
好ましくは、原料粉体中の粒径０．５μｍ以下の粒子の
含有率が０．０３重量％以上であれば、粉体取り扱い性
を著しく改良することができる。The influence of the particle size distribution of the polyphenylene ether resin as a raw material on the particle size distribution of the powder obtained by the method of the present invention is small. Therefore, a raw material powder containing a larger amount of fine particles has a greater effect of improving the powder handling property. It is preferable that particles having a particle diameter of 0.5 μm or less contained in the raw material powder account for 0.005% by weight or more of the whole. More preferably, when the content of particles having a particle size of 0.5 μm or less in the raw material powder is 0.03% by weight or more, the powder handling properties can be significantly improved.
【００１９】また、本発明で使用する成型装置は、例え
ば圧縮ロールタイプ、ブリケッティングロールタイプ、
打錠成型タイプ等の圧縮成型機が挙げられる。５〜２０
０℃の温度範囲で密度が０．７〜１．０５５ｇ／ｃｍ3
になるまでの加圧が可能であれば、本発明の効果は充分
に得られる。The molding apparatus used in the present invention is, for example, a compression roll type, a briquetting roll type,
A compression molding machine such as a tablet molding type is exemplified. 5-20
The density is 0.7 to 1.055 g / cm 3 in the temperature range of 0 ° C.
As long as the pressure can be increased up to, the effect of the present invention can be sufficiently obtained.
【００２０】また、本発明で使用する粉砕装置は、粗砕
機、中間粉砕機、微粉砕機が挙げられる。粗砕機の例
は、ジョークラッシャー、ジャイレイトリークラッシャ
ー、シュレッター等が挙げられる。中間粉砕機の例は、
ハンマーミルやディスインテグレーター等の衝撃粉砕
機、ロール粉砕機、エッジランナー等が挙げられる。微
粉砕機の例は、遠心力粉砕機、ボールミル、振動ミル、
コロイドミルやつき臼、ひき臼等が挙げられる。The pulverizer used in the present invention includes a coarse pulverizer, an intermediate pulverizer and a fine pulverizer. Examples of the crusher include a jaw crusher, a gyratory crusher, a Schletter, and the like. An example of an intermediate crusher is
Examples include impact crushers such as hammer mills and disintegrators, roll crushers, and edge runners. Examples of fine mills include centrifugal mills, ball mills, vibratory mills,
A colloid mill, a mortar, a mill, and the like can be used.
【００２１】従来の方法では強度の低い圧縮成型体しか
得られず実用に耐えなかったが、本発明により充分な強
度を持った成型体を得ることが可能になった。その結
果、成型後に粉砕工程を加えることにより、微粒子を大
幅に低減した取り扱いやすい粒径分布を持ったポリフェ
ニレンエーテル粉体を得ることが可能になった。According to the conventional method, only a low-strength compression molded article was obtained, which was not practical. However, the present invention has made it possible to obtain a molded article having sufficient strength. As a result, it became possible to obtain a polyphenylene ether powder having a particle size distribution that was easy to handle and in which the fine particles were significantly reduced by adding a pulverizing step after molding.
【００２２】圧縮成型時の粉体の温度範囲は５〜２００
℃であることが必要である。５℃未満では充分な強度を
持った成型体が得られない。２００℃を越えると、ポリ
フェニレンエーテル中に含まれるアミンが離脱し、加工
時に品質の低下をもたらす。更に好ましくは、圧縮成型
時の温度範囲を８０℃以上１６５℃以下にすれば、より
強固で、品質的にも優れた成型体を得ることができる。The temperature range of the powder during compression molding is 5 to 200.
It must be in ° C. If the temperature is lower than 5 ° C., a molded product having sufficient strength cannot be obtained. When the temperature exceeds 200 ° C., the amine contained in the polyphenylene ether is released, resulting in deterioration in quality during processing. More preferably, if the temperature range at the time of compression molding is set to 80 ° C. or more and 165 ° C. or less, a stronger and more excellent molded product can be obtained.
【００２３】本発明では成型体の密度を、０．７〜１．
０５５ｇ／ｃｍ3の範囲にすることが必要である。成型
体の密度が０．７ｇ／ｃｍ3未満であれば、成型体に充
分な強度を保有させることができず、再粉砕を実施した
ときに多量の微小粒子を発生してしまう。また、成型体
の密度が１．０５５ｇ／ｃｍ3を超えて圧縮すると、成
型時のせん断により局部熱が発生し、成型体が溶融し、
再粉砕時に多大なエネルギーが必要となるとともに多量
の微小粒子を発生させてしまう。また、せん断熱によ
り、ポリフェニレンエーテルに含まれるアミンが離脱
し、加工時に品質低下をもたらす。更に好ましくは、
０．７５〜１．０４ｇ／ｃｍ3であれば、成型体は局部
的なせん断熱を受けず、溶融部の少ない強固な粉の凝集
体として取り出すことができる。これを再粉砕すること
により、良好な粉体特性を備えた粉体を得ることができ
る。In the present invention, the density of the molded body is set to 0.7 to 1.
It is necessary to be in the range of 055 g / cm 3 . If the density of the molded body is less than 0.7 g / cm 3 , the molded body cannot have sufficient strength, and a large amount of fine particles will be generated when re-grinding is performed. Further, when the density of the molded body is compressed to exceed 1.055 g / cm 3 , local heat is generated by shearing during molding, and the molded body is melted.
A large amount of energy is required at the time of re-grinding, and a large amount of fine particles are generated. In addition, the amine contained in the polyphenylene ether is released due to the shearing heat, and the quality is reduced during processing. More preferably,
When it is 0.75 to 1.04 g / cm 3 , the molded body does not receive local shearing heat and can be taken out as an aggregate of strong powder with a small number of melted parts. By re-grinding the powder, a powder having good powder characteristics can be obtained.
【００２４】再粉砕は、前記の装置を用いて実施するこ
とができ、再粉砕により粒径１μｍ以下の微小粒子の含
有量を全体の０．５重量％以下に低減することができ
る。そして、好ましくは同時に３μ〜５ｍｍの粒子の比
率を全体の９０重量％以上とする。The re-grinding can be carried out using the above-mentioned apparatus, and the content of the fine particles having a particle size of 1 μm or less can be reduced to 0.5% by weight or less of the whole by the re-grinding. Preferably, the ratio of the particles having a size of 3 to 5 mm is simultaneously set to 90% by weight or more of the whole.
【００２５】[0025]
【発明の実施の形態】次に実施例により本発明を更に詳
細に説明するが、本発明はこれらの例によってなんら限
定されるものではない。Now, the present invention will be described in further detail with reference to Examples. However, it should be understood that the present invention is by no means restricted by such specific Examples.
【００２６】[0026]
【実施例１〜４】本テスト原料は、嵩密度０．５２７、
固有粘度（クロロホルム中、３０℃）が０．５３、粒径
１００μｍ以下の粒子の含有率が６０重量％、１０μｍ
以下の粒子の含有率が１２重量％、０．５μｍ以下の粒
子の含有率が０．０９重量％のポリ（２，６ジメチル−
１，４−フェニレン）エーテル（以後ＰＰＥとする）の
粉体を使用した。成型装置は、直径：２５８ｍｍ×幅：
３８ｍｍのロールを有するローラーコンパクタを使用し
た。ローラーコンパクタは２個のロールを有し、供給部
に設置したスクリューでロール間にPPE粉体を押し込
み、ロール部で圧縮し、板状の成型体を得る。また、粉
砕は、ハンマーミルタイプの粉砕機を使用した。粉砕機
での粒径調整はハンマーミルに付設したスクリーンによ
り、５ｍｍ径以下の粉体を排出する形式とした。Examples 1-4 The test raw materials had a bulk density of 0.527,
The intrinsic viscosity (in chloroform, 30 ° C.) is 0.53, and the content of particles having a particle size of 100 μm or less is 60% by weight and 10 μm.
The content of the following particles is 12% by weight, and the content of the particles having a particle size of 0.5 μm or less is 0.09% by weight.
A powder of 1,4-phenylene) ether (hereinafter referred to as PPE) was used. The molding device has a diameter of 258 mm and a width of:
A roller compactor with a 38 mm roll was used. The roller compactor has two rolls, and PPE powder is pushed between the rolls by a screw installed in a supply unit, and compressed by the rolls to obtain a plate-like molded body. For the pulverization, a hammer mill type pulverizer was used. The particle size was adjusted by a pulverizer by discharging a powder having a diameter of 5 mm or less through a screen attached to a hammer mill.
【００２７】ローラーコンパクタを用いて、以下の成型
を行った。 (1)温度：１２０℃、成型体密度：０．７９５ｇ／ｃｍ3
（成型圧：３０ｋｇ／ｃｍ2） (2)温度：１２０℃、成型体密度：０．８２０ｇ／ｃｍ3
（成型圧：４０ｋｇ／ｃｍ2） (3)温度：１２０℃、成型体密度：０．８４５ｇ／ｃｍ3
（成型圧：５０ｋｇ／ｃｍ2） (4)温度：１２０℃、成型体密度：０．８９５ｇ／ｃｍ3
（成型圧：７０ｋｇ／ｃｍ2） 得られた成型体は、(1)，(2)，(3)は白色の凝集体であ
り、(4)は一部が半透明化した溶融体を含む凝集体であ
った。更に、この成型体を粉砕した結果、得られた粉粒
体中の小粒子含有量は以下の通りであった。The following molding was performed using a roller compactor. (1) Temperature: 120 ° C., density of molded body: 0.795 g / cm 3
(Molding pressure: 30 kg / cm 2 ) (2) Temperature: 120 ° C., density of molded body: 0.820 g / cm 3
(Molding pressure: 40 kg / cm 2 ) (3) Temperature: 120 ° C., density of molded body: 0.845 g / cm 3
(Molding pressure: 50 kg / cm 2 ) (4) Temperature: 120 ° C., density of molded body: 0.895 g / cm 3
(Molding pressure: 70 kg / cm 2 ) In the obtained molded body, (1), (2) and (3) are white aggregates, and (4) contains a partially translucent melt. It was an aggregate. Furthermore, as a result of pulverizing this molded product, the content of small particles in the obtained powdery granules was as follows.
【００２８】[0028]
【表１】 [Table 1]
【００２９】[0029]
【実施例５】成型条件を、 (5)温度：１６０℃、成型体密度：１．０３１ｇ／ｃｍ3
（成型圧：１６０ｋｇ／ｃｍ2） とし、また成型装置はロール部に直径５ｍｍの窪みを有
するブリケットロールとしたこと以外は、実施例１〜４
と全く同様の操作を実施した。得られた成型体は、一部
が半透明化した溶融体であった。更に、この成型体を実
施例１〜４と同様の方法で粉砕した結果、得られた粉粒
体中の小粒子含有量は以下の通りであった。Embodiment 5 The molding conditions were as follows: (5) Temperature: 160 ° C., Density of molded body: 1.031 g / cm 3
(Molding pressure: 160 kg / cm 2 ), and the molding apparatus was a briquette roll having a recess having a diameter of 5 mm in the roll part.
The same operation as described above was performed. The obtained molded body was a melt partially translucent. Furthermore, as a result of pulverizing this molded product in the same manner as in Examples 1 to 4, the content of small particles in the obtained granules was as follows.
【００３０】[0030]
【表２】 [Table 2]
【００３１】[0031]
【比較例１，２】成型条件を、 (6)温度：１２０℃、成型体密度：０．６５０ｇ／ｃｍ3
（成型圧：５ｋｇ／ｃｍ2） (7)温度：１６０℃、成型体密度：０．６８５ｇ／ｃｍ3
（成型圧：５ｋｇ／ｃｍ2） としたこと以外は、実施例１〜４と全く同様の操作を実
施した。得られた成型体は、(6)，(7)とも白色の凝集体
であった。これらは何れの成型体も罅を生じており、手
でも容易に割れる状態であった。更に、この成型体を実
施例１〜４と同様の方法で粉砕した結果、得られた粉粒
体中の小粒子含有量は以下の通りであった。Comparative Examples 1 and 2 The molding conditions were as follows: (6) Temperature: 120 ° C., Density of molded body: 0.650 g / cm 3
(Molding pressure: 5 kg / cm 2 ) (7) Temperature: 160 ° C., density of molded body: 0.685 g / cm 3
(Molding pressure: 5 kg / cm 2 ) Except that the operation was the same as in Examples 1-4. The obtained molded product was a white aggregate in both (6) and (7). All of these molded articles had cracks, and were easily broken by hand. Furthermore, as a result of pulverizing this molded product in the same manner as in Examples 1 to 4, the content of small particles in the obtained granules was as follows.
【００３２】[0032]
【表３】 [Table 3]
【００３３】成型体密度が０．７ｇ／ｃｍ3以下である
と、充分な強度を持った成型体は得られない。この結
果、粉砕により１０μｍ以下の小粒子が発生し、粉体取
り扱い性の改良効果は小さい。If the density of the molded body is 0.7 g / cm 3 or less, a molded body having sufficient strength cannot be obtained. As a result, small particles of 10 μm or less are generated by the pulverization, and the effect of improving the powder handling property is small.
【００３４】[0034]
【比較例３，４】成型条件を、 (8)温度：３℃、成型体密度：０．６０５ｇ／ｃｍ3（成
型圧：７０ｋｇ／ｃｍ2） (9)温度：３℃（成型圧：４ｋｇ／ｃｍ2） としたこと以外は、実施例１〜４と全く同様の操作を実
施した。得られた成型体は、(8)は白色の凝集体であ
り、罅を生じており、手でも容易に崩れる状態であっ
た。(9)は、密度０．５５０ｇ／ｃｍ3程度の成型体生成
を試みたが、成型圧を下げると原料パウダーはロール間
を素抜けてしまい、目標密度の成型体は得られなかっ
た。更に、(8)で得られた成型体を実施例１〜４と同様
の方法で粉砕した結果、得られた粉粒体中の小粒子含有
量は以下の通りであった。Comparative Examples 3 and 4 The molding conditions were as follows: (8) Temperature: 3 ° C., Density of molded body: 0.605 g / cm 3 (molding pressure: 70 kg / cm 2 ) (9) Temperature: 3 ° C. (molding pressure: 4 kg) / Cm 2 ), except that the operation was the same as in Examples 1 to 4. In the obtained molded body, (8) was a white agglomerate, had a crack, and was easily broken by hand. For (9), an attempt was made to produce a molded body having a density of about 0.550 g / cm 3. However, when the molding pressure was lowered, the raw material powder was able to pass through between the rolls, and a molded body having the target density could not be obtained. Furthermore, as a result of grinding the molded product obtained in (8) in the same manner as in Examples 1 to 4, the content of small particles in the obtained powdery granules was as follows.
【００３５】[0035]
【表４】 [Table 4]
【００３６】成型温度を５℃以下にすると、成型体の密
度が上がらず、充分な強度を持った成型体は得られな
い。低密度の成型体を狙うと、成型体すら得られない場
合もある。成型体が得られた場合でも、粉砕により１０
μｍ以下の小粒子が発生し、原料と大差のない粉体に戻
ってしまう。When the molding temperature is 5 ° C. or lower, the density of the molded body does not increase, and a molded body having sufficient strength cannot be obtained. Aiming at a low-density molded product may not even provide a molded product. Even if a molded body is obtained, it is possible to obtain 10
Small particles of less than μm are generated, and the powder returns to a powder that is not much different from the raw material.
【００３７】[0037]
【比較例５】成型条件を、 (10)温度：１７０℃、成型体密度：１．０５９ｇ／ｃｍ
3（成型圧：４２０ｋｇ／ｃｍ2） としたこと以外は、実施例１〜４と全く同様の操作を実
施した。ロールより排出された成型体は茶褐色の溶融体
であり、成型後冷却すると非常に強固な固まりとなっ
た。更に、この成型体に対し実施例１〜４と同様の方法
で粉砕を試みたが、粉砕機のスクリーン上に粉砕不能な
固まりが多数残った。スクリーン上に残った粉砕不能物
は、粉砕機フィードに対して３３．４重量％であった。Comparative Example 5 The molding conditions were as follows: (10) Temperature: 170 ° C., Density of molded body: 1.059 g / cm
Except that the pressure was set to 3 (molding pressure: 420 kg / cm 2 ), the same operation as in Examples 1 to 4 was performed. The molded body discharged from the roll was a brown-colored melt, and when cooled after molding, it became a very strong lump. Further, pulverization of this molded body was attempted in the same manner as in Examples 1 to 4, but a large number of unpulverizable clusters remained on the screen of the pulverizer. The non-millable material remaining on the screen was 33.4% by weight based on the mill feed.
【００３８】[0038]
【発明の効果】以上に述べたように、本発明の方法によ
りポリフェニレンエーテル樹脂粉体から微小粒子を著し
く減らすことができ、粉体特性が優れ、取り扱いやす
く、押し出し生産性の高い粉体に簡便に改良できる。As described above, according to the method of the present invention, fine particles can be remarkably reduced from the polyphenylene ether resin powder, the powder characteristics are excellent, the handling is easy, and the powder having high extrusion productivity is easily obtained. Can be improved.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 栗原 哲男 千葉県袖ケ浦市中袖５番地１ 旭化成工業 株式会社内 Ｆターム(参考） 4F070 AA52 DA08 DA43 DA46 DA50 DA52 DC07 DC08 4F201 AA32 AC04 AR12 AR15 BA04 BC01 BC12 BC15 BL03 BL05 BM07 BN29 BN32 ────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Tetsuo Kurihara 5-1, Nakasode, Sodegaura-shi, Chiba F-term (reference) 4A070 DA50 DA08 DA43 DA46 DA50 DA52 DC07 DC08 4F201 AA32 AC04 AR12 AR15 BA04 BC01 BC12 BC15 BL03 BL05 BM07 BN29 BN32
Claims (3)
ンエーテル粉体を圧縮成型することにより密度０．７〜
１．０５５ｇ／ｃｍ3の成型体を生成し、得られた成型
体を再粉砕することによって粒径１μｍ以下の微小粒子
の含有率を全体の０．５重量％以下とすることを特徴と
する粒度分布の改良されたポリフェニレンエーテル粉体
の製造法。1. A polyphenylene ether powder having a temperature of 5 to 200 ° C. is subjected to compression molding to obtain a density of 0.7 to
A molded body of 1.055 g / cm 3 is produced, and the obtained molded body is reground to reduce the content of fine particles having a particle diameter of 1 μm or less to 0.5% by weight or less of the whole. A method for producing a polyphenylene ether powder having an improved particle size distribution.
径３μｍ〜５ｍｍの粒子の比率が全体の９０重量％以上
である請求項１記載の粒度分布の改良されたポリフェニ
レンエーテル粉体の製造法。2. The polyphenylene ether powder having an improved particle size distribution according to claim 1, wherein the proportion of particles having a particle size of 3 μm to 5 mm present in the powder obtained by re-grinding the molded body is 90% by weight or more. Manufacturing method.
ル粉体中に粒子径０．５μｍ以下の微小粒子が０．００
５重量％以上存在する請求項１記載の粒度分布の改良さ
れたポリフェニレンエーテル粉体の製造法。3. The polyphenylene ether powder before compression molding contains fine particles having a particle diameter of 0.5 μm or less in the polyphenylene ether powder.
The method for producing a polyphenylene ether powder having an improved particle size distribution according to claim 1, which is present in an amount of 5% by weight or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10965899A JP4152521B2 (en) | 1999-04-16 | 1999-04-16 | Production method of polyphenylene ether powder with improved particle size distribution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10965899A JP4152521B2 (en) | 1999-04-16 | 1999-04-16 | Production method of polyphenylene ether powder with improved particle size distribution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000302877A true JP2000302877A (en) | 2000-10-31 |
| JP4152521B2 JP4152521B2 (en) | 2008-09-17 |
Family
ID=14515883
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10965899A Expired - Lifetime JP4152521B2 (en) | 1999-04-16 | 1999-04-16 | Production method of polyphenylene ether powder with improved particle size distribution |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001172397A (en) * | 1999-12-17 | 2001-06-26 | Kureha Chem Ind Co Ltd | Method for producing resin composition pellet |
| JP2008524356A (en) * | 2004-12-21 | 2008-07-10 | エボニック デグサ ゲーエムベーハー | Fine-grained polyarylene ether ketone powder |
| US7947204B2 (en) * | 2004-04-16 | 2011-05-24 | Sabic Innovative Plastics Ip B.V. | Poly(arylene ether) compression molding |
| CN103421178A (en) * | 2012-05-17 | 2013-12-04 | 旭化成化学株式会社 | Production method for polyphenylene ether powder |
| JP2017160399A (en) * | 2016-03-11 | 2017-09-14 | 旭化成株式会社 | Polyphenylene ether powder having micro-voids and manufacturing method of the same |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6581064B2 (en) | 2016-10-28 | 2019-09-25 | 旭化成株式会社 | Polyphenylene ether powder and production method |
-
1999
- 1999-04-16 JP JP10965899A patent/JP4152521B2/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001172397A (en) * | 1999-12-17 | 2001-06-26 | Kureha Chem Ind Co Ltd | Method for producing resin composition pellet |
| JP4563536B2 (en) * | 1999-12-17 | 2010-10-13 | 株式会社クレハ | Method for producing resin composition pellets |
| US7947204B2 (en) * | 2004-04-16 | 2011-05-24 | Sabic Innovative Plastics Ip B.V. | Poly(arylene ether) compression molding |
| US8703028B2 (en) | 2004-04-16 | 2014-04-22 | Sabic Innovative Plastics Ip B.V. | Poly(arylene ether) compression molding |
| EP1742998B1 (en) * | 2004-04-16 | 2017-10-18 | SABIC Global Technologies B.V. | Polyarylene ether compression molding |
| JP2008524356A (en) * | 2004-12-21 | 2008-07-10 | エボニック デグサ ゲーエムベーハー | Fine-grained polyarylene ether ketone powder |
| JP4922183B2 (en) * | 2004-12-21 | 2012-04-25 | エボニック デグサ ゲーエムベーハー | Fine-grained polyarylene ether ketone powder |
| CN103421178A (en) * | 2012-05-17 | 2013-12-04 | 旭化成化学株式会社 | Production method for polyphenylene ether powder |
| JP2017160399A (en) * | 2016-03-11 | 2017-09-14 | 旭化成株式会社 | Polyphenylene ether powder having micro-voids and manufacturing method of the same |
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