JP2012030471A - Method of manufacturing thin-wall intermediate molding - Google Patents
Method of manufacturing thin-wall intermediate molding Download PDFInfo
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本発明は、ポリフェニレンスルフィド（ＰＰＳ）の性質を利用した各種製品の製造中間体として好適な薄肉の中間成形品の製造方法に関する。 The present invention relates to a method for producing a thin intermediate molded article suitable as a production intermediate for various products utilizing the properties of polyphenylene sulfide (PPS).
ＰＰＳ及び無機充填剤を含む樹脂組成物は、成形物が優れた機械的性質、耐熱性、耐薬品性、電気特性を有するため、自動車、電気・電子部品、化学機器等の部品材料として汎用されている。 Resin compositions containing PPS and inorganic fillers are widely used as component materials for automobiles, electrical / electronic components, chemical equipment, etc., because molded products have excellent mechanical properties, heat resistance, chemical resistance, and electrical properties. ing.
ＰＰＳからなる成形品では、ＰＰＳの結晶化度が高いと二次加工が困難になるため、二次加工するときは、溶融させることで結晶化度を下げる必要がある。そうすると、工数も増加し、消費エネルギーも増加するため、製造効率が低下してしまい、二酸化炭素の排出量の増加にもつながる。 In a molded product made of PPS, secondary processing becomes difficult if the crystallinity of PPS is high. Therefore, when performing secondary processing, it is necessary to lower the crystallinity by melting. If it does so, since man-hours will increase and energy consumption will also increase, manufacturing efficiency will fall and it will also lead to the increase in the discharge | emission amount of a carbon dioxide.
特許文献１、２では、高い結晶化度のＰＰＳからなる樹脂成形品の製造方法が開示されている。 Patent Documents 1 and 2 disclose a method for producing a resin molded product made of PPS having a high crystallinity.
本発明は、ＰＰＳの結晶化度を低く抑えることで、最終製品を得るための二次加工が容易になり、製造効率を高めることで、二酸化炭素の排出量の減少ができる、ＰＰＳの性質を利用した各種製品の製造中間体として好適な薄肉の中間成形品の製造方法を提供することを課題とする。 The present invention makes it possible to facilitate the secondary processing for obtaining the final product by suppressing the crystallinity of the PPS to be low, and to reduce the carbon dioxide emission by increasing the production efficiency. It is an object of the present invention to provide a method for producing a thin intermediate molded article suitable as a production intermediate for various products used.
本願請求項１の発明は、課題の解決手段として、
非晶状態のポリフェニレンスルフィド（ＰＰＳ）を含む樹脂組成物からなるシートを得る工程、
前記シートをＰＰＳのガラス転移温度（Tg）＋２０℃以上の温度から、冷結晶化温度（Tcc）＋１０℃以下の温度に予熱する工程、
予熱したシートを１０〜１５０℃に設定した金型内に入れて熱成形した後、さらに前記温度範囲で保持してＰＰＳの結晶化度が２０％以下である薄肉成形品を得る工程、
を有している薄肉の中間成形品の製造方法を提供する。
The invention of claim 1 of the present application is as means for solving the problems.
Obtaining a sheet comprising a resin composition containing amorphous polyphenylene sulfide (PPS);
Preheating the sheet from a glass transition temperature (Tg) of PPS + 20 ° C. or higher to a temperature of cold crystallization temperature (Tcc) + 10 ° C. or lower;
A step of obtaining a thin-walled molded article having a PPS crystallinity of 20% or less by holding the preheated sheet in a mold set at 10 to 150 ° C. and thermoforming, and further holding in the temperature range;
A method for producing a thin intermediate molded article having
本願請求項２の発明は、課題の他の解決手段として、
結晶状態のポリフェニレンスルフィド（ＰＰＳ）を含む樹脂組成物からなるシートを得る工程、
前記シートをＰＰＳの融点（Tm）−４０℃以上から融点（Tm）−２０℃までの温度で予熱する工程、
予熱したシートを１０〜１５０℃に設定した金型内に入れて熱成形した後、さらに前記温度範囲で保持してＰＰＳの結晶化度が２０％以下である薄肉の中間成形品を得る工程、
を有している薄肉の中間成形品の製造方法を提供する。
The invention of claim 2 of the present application is another means for solving the problems.
Obtaining a sheet comprising a resin composition containing polyphenylene sulfide (PPS) in a crystalline state;
Preheating the sheet at a temperature from the melting point (Tm) of -40 ° C. or higher to the melting point (Tm) of -20 ° C .;
A step of obtaining a thin intermediate molded product having a PPS crystallinity of 20% or less by holding the preheated sheet in a mold set at 10 to 150 ° C. and thermoforming, and further holding in the above temperature range;
A method for producing a thin intermediate molded article having
本発明の製造方法により得られる薄肉の中間成形品は、結晶化度が２０％以下であることから二次加工が容易である。 Since the thin intermediate molded product obtained by the production method of the present invention has a crystallinity of 20% or less, secondary processing is easy.
（１）第１の製造方法
最初の工程にて、非晶状態のポリフェニレンスルフィド（ＰＰＳ）を含む樹脂組成物からなるシートを得る。
(1) First Production Method In the first step, a sheet made of a resin composition containing amorphous polyphenylene sulfide (PPS) is obtained.
この工程は、例えば押出機とＴダイを組み合わせた公知の方法（例えば特許文献２の実施例に記載の方法）を適用してシートを得ることができる。 In this step, for example, a known method (for example, a method described in Examples in Patent Document 2) in which an extruder and a T die are combined can be applied to obtain a sheet.
本発明で用いる樹脂組成物に含まれるＰＰＳは、ホモポリマーでもよいし、コポリマーでもよい。ホモポリマーの場合は線状ポリマーが好ましい。 The PPS contained in the resin composition used in the present invention may be a homopolymer or a copolymer. In the case of a homopolymer, a linear polymer is preferable.
コポリマーは、ｐ−フェニレン基を含む構成単位と、他のアリーレン基（好ましくはｍ−フェニレン基）を含む構成単位のコポリマーを挙げることができるが、成形性、耐熱性、機械的特性の点から、ｐ−フェニレン基を含む構成単位の比率が６０モル％以上のものが好ましく、７０モル％以上のものがより好ましい。コポリマーは、ランダム結合でも、ブロック結合でもよいが、ブロック結合のものの方が、耐熱性、機械的特性の点から好ましい。 Examples of the copolymer include a copolymer of a structural unit containing a p-phenylene group and a structural unit containing another arylene group (preferably m-phenylene group). From the viewpoint of moldability, heat resistance, and mechanical properties. The proportion of structural units containing a p-phenylene group is preferably 60 mol% or more, more preferably 70 mol% or more. The copolymer may be a random bond or a block bond, but a block bond is preferred from the viewpoint of heat resistance and mechanical properties.
ＰＰＳ（ホモポリマー又はコポリマー）は、溶融粘度（測定条件：温度310℃，剪断速度1200ｓ-1）が３５０〜１０００Pa・sであり、好ましくは４５０〜６００Pa・sである。 PPS (homopolymer or copolymer) has a melt viscosity (measurement conditions: temperature 310 ° C., shear rate 1200 s −1 ) of 350 to 1000 Pa · s, preferably 450 to 600 Pa · s.
本発明で用いる樹脂組成物には、必要に応じて、本発明の課題を解決できる範囲の量及び種類の熱可塑性を配合することができる。
このような熱可塑性樹脂はＰＰＳよりも融点が低いものが好ましく、ポリエチレン、ポリプロピレン又はこれらの変性重合体等のポリオレフィンを主体とするオレフィン系重合体又は共重合体；ナイロン６、ナイロン６６、その他のポリアミド系重合体又は共重合体；ポリエチレンテレフタレート、ポリブチレンテレフタレート等を主体とするポリエステル重合体又は共重合体；液晶性ポリエステル重合体；ポリスチレン、ポリアクリロニトリル、ＡＢＳ等のスチレン系重合体；ポリアルキルアクリレート等のアクリル系重合体；ポリカーボネート、ポリフェニレンオキサイド、ポリアセタール等を挙げることができる。これらの熱可塑性樹脂は、２種以上を使用することができる。
If necessary, the resin composition used in the present invention can be blended with an amount and a kind of thermoplasticity within a range that can solve the problems of the present invention.
Such a thermoplastic resin preferably has a melting point lower than that of PPS, and is an olefin polymer or copolymer mainly composed of polyolefin such as polyethylene, polypropylene or a modified polymer thereof; nylon 6, nylon 66, other Polyamide polymer or copolymer; Polyester polymer or copolymer mainly composed of polyethylene terephthalate, polybutylene terephthalate, etc .; Liquid crystalline polyester polymer; Styrene polymer such as polystyrene, polyacrylonitrile, ABS; Polyalkyl acrylate And acrylic polymers such as polycarbonate, polyphenylene oxide, polyacetal and the like. Two or more of these thermoplastic resins can be used.
本発明で用いる樹脂組成物には、薄肉成形品に要求される性質等に応じて、粒状、繊維状又はフレーク状（板状）充填材から選ばれる１種又は２種以上を配合することができる。 The resin composition used in the present invention may contain one or more selected from granular, fibrous or flaky (plate-like) fillers depending on the properties required for the thin molded article. it can.
繊維状充填材としては、ガラス繊維、カーボン繊維、シリカ繊維、シリカ・アルミナ繊維、ジルコニウム繊維、窒化硼素繊維、窒化珪素繊維、硼素繊維、チタン酸カリウム繊維のほか、ステンレス、アルミニウム、チタン、銅、黄銅等の繊維を挙げることができ、これらの中でも、ガラス繊維、カーボン繊維が好ましい。 Examples of the fibrous filler include glass fiber, carbon fiber, silica fiber, silica / alumina fiber, zirconium fiber, boron nitride fiber, silicon nitride fiber, boron fiber, potassium titanate fiber, stainless steel, aluminum, titanium, copper, Examples thereof include fibers such as brass, and among these, glass fibers and carbon fibers are preferable.
繊維状充填材は、平均繊維長が１〜８００μmのものが好ましく、より好ましくは５〜６００μmのものである。前記範囲のものを用いると、薄肉成形品の寸法安定性が良くなり、外観も良くなる。平均繊維長さは、計数法（走査型電子顕微鏡で観察し、充填材の大きさを測定する方法）によって求める。 The fibrous filler preferably has an average fiber length of 1 to 800 μm, more preferably 5 to 600 μm. When the product within the above range is used, the dimensional stability of the thin molded product is improved and the appearance is also improved. The average fiber length is determined by a counting method (a method of observing with a scanning electron microscope and measuring the size of the filler).
粒状充填材としては、カーボンブラック、黒鉛、シリカ、石英粉末、ガラスビーズ、ガラス粉、珪酸カルシウム、珪酸アルミニウム、カオリン、タルク、クレー、珪藻土、ウォラストナイトのような珪酸塩、酸化鉄、酸化チタン、アルミナのような金属の酸化物、炭酸カルシウム、炭酸マグネシウムのような金属の炭酸塩、硫酸カルシウム、硫酸バリウムのような金属の硫酸塩、その他、炭化珪素、窒化珪素、窒化硼素、各種金属粉末等を挙げることができる。 As granular fillers, carbon black, graphite, silica, quartz powder, glass beads, glass powder, calcium silicate, aluminum silicate, kaolin, talc, clay, diatomaceous earth, silicates such as wollastonite, iron oxide, titanium oxide Metal oxides such as alumina, metal carbonates such as calcium carbonate and magnesium carbonate, metal sulfates such as calcium sulfate and barium sulfate, silicon carbide, silicon nitride, boron nitride, various metal powders Etc.
粒状充填材は、平均粒径が１〜８００μmのものが好ましく、より好ましくは５〜６００μmのものである。前記範囲のものを用いると、薄肉成形品の寸法安定性が良くなり、外観も良くなる。平均粒径は、計数法（走査型電子顕微鏡で観察し、充填材の大きさを測定する方法）によって求める。 The granular filler preferably has an average particle diameter of 1 to 800 μm, more preferably 5 to 600 μm. When the product within the above range is used, the dimensional stability of the thin molded product is improved and the appearance is also improved. The average particle diameter is determined by a counting method (a method of observing with a scanning electron microscope and measuring the size of the filler).
フレーク状充填材としては、マイカ、ガラスフレーク、各種金属箔等を挙げることができる。 Examples of the flaky filler include mica, glass flakes and various metal foils.
フレーク状充填材は、平均最大長さが１〜８００μmのものが好ましく、より好ましくは５〜６００μmのものである。前記範囲のものを用いると、薄肉成形品の寸法安定性が良くなり、外観も良くなる。平均最大長さは、計数法（走査型電子顕微鏡で観察し、充填材の大きさを測定する方法）によって求める。 The flaky filler preferably has an average maximum length of 1 to 800 μm, more preferably 5 to 600 μm. When the product within the above range is used, the dimensional stability of the thin molded product is improved and the appearance is also improved. The average maximum length is obtained by a counting method (a method of observing with a scanning electron microscope and measuring the size of the filler).
これらの充填材は、必要に応じて、次亜燐酸又はその塩を表面に付着させたものを用いてもよく、収束剤を用いて収束したものを用いてもよく、表面処理剤（エポキシ系化合物、イソシアナート系化合物、シラン系化合物、チタネート系化合物）を用いて表面処理したものを用いてもよい。 As necessary, these fillers may be prepared by adhering hypophosphorous acid or a salt thereof to the surface, or may be converged by using a sizing agent. Compounds, isocyanate compounds, silane compounds, titanate compounds) that have been surface-treated may be used.
これらの充填材の配合量は、ＰＰＳ１００質量部に対して１〜２００質量部が好ましく、５〜１００質量部がより好ましく、１０〜５０質量部が更に好ましい。 1-200 mass parts is preferable with respect to 100 mass parts of PPS, as for the compounding quantity of these fillers, 5-100 mass parts is more preferable, and 10-50 mass parts is still more preferable.
また、上記充填材とは別に、必要に応じて有機質充填材を補助的に配合することができる。有機質充填材としては、フッ素樹脂、芳香族ポリアミド等の高融点の繊維状又は粉粒状の重合体を用いることができる。 In addition to the filler, an organic filler can be supplementarily blended as necessary. As the organic filler, a high melting point fibrous or powdery polymer such as fluororesin and aromatic polyamide can be used.
また樹脂組成物には、最終製品の用途に応じて、各種添加剤、例えば、顔料、紫外線吸収剤、酸化防止剤、熱安定剤、滑剤、難燃剤、離型剤、その他の公知の添加剤を配合することができる。 In the resin composition, various additives such as pigments, ultraviolet absorbers, antioxidants, heat stabilizers, lubricants, flame retardants, release agents, and other known additives are used depending on the use of the final product. Can be blended.
次の工程にて、前工程で得られたシートをＰＰＳのガラス転移温度（Tg）＋２０℃以上の温度から、冷結晶化温度（Tcc）＋１０℃以下の温度に予熱する。 In the next step, the sheet obtained in the previous step is preheated from a glass transition temperature (Tg) of PPS + 20 ° C. or higher to a temperature of cold crystallization temperature (Tcc) + 10 ° C. or lower.
この予熱は、次工程で使用する成形機（真空成形機又は圧空成形機等）により行うことができる。
予熱温度は、Ｔｇ＋２５℃からＴcc＋５℃以下の温度範囲が好ましい。予熱時間は、シートが上記温度範囲になるまでの時間である。
This preheating can be performed by a molding machine (such as a vacuum molding machine or a pressure molding machine) used in the next step.
The preheating temperature is preferably in the temperature range of Tg + 25 ° C. to Tcc + 5 ° C. or less. The preheating time is the time until the sheet reaches the above temperature range.
予熱温度が前記下限値以上であると、寸法精度良く中間成形品を得ることができ、予熱温度が前記上限値以下であると、成形時のドローダウンが防止できる。 When the preheating temperature is equal to or higher than the lower limit value, an intermediate molded product can be obtained with high dimensional accuracy, and when the preheating temperature is equal to or lower than the upper limit value, drawdown during molding can be prevented.
次の工程にて、予熱したシートを１０〜１５０℃に設定した金型内に入れて熱成形した後、さらに前記温度範囲で保持してＰＰＳの結晶化度が２０％以下である薄肉の中間成形品を得る。前記温度範囲は３０〜８０℃が好ましい。 In the next step, after the preheated sheet is put in a mold set at 10 to 150 ° C. and thermoformed, it is further held in the above temperature range, and the middle of the thin wall where the crystallinity of PPS is 20% or less Get a molded product. The temperature range is preferably 30 to 80 ° C.
金型温度が前記下限値以上であると、寸法精度良く薄肉の中間形品を得ることができ、金型温度が前記上限値以下であると、ＰＰＳが結晶化度２０％以下に結晶化される。 If the mold temperature is equal to or higher than the lower limit, a thin intermediate product can be obtained with good dimensional accuracy. If the mold temperature is equal to or lower than the upper limit, PPS is crystallized to a crystallinity of 20% or lower. The
薄肉の中間成形品の結晶化度は、２０％以下であり、０％（非晶状態）でもよい。 The crystallinity of the thin intermediate molded product is 20% or less, and may be 0% (amorphous state).
薄肉の中間成形品の厚みは、二次加工品の形態に応じて適宜決定することができる。 The thickness of the thin intermediate molded product can be appropriately determined according to the form of the secondary processed product.
中間成形品の形状は、目的とする二次加工に対応した形状にすることができる。例えば、底の浅いトレー、前記トレーの開口部にフランジ（鍔）が付いたもの、円筒、深絞り成形品（絞り比が１以上）にすることができる。 The shape of the intermediate molded product can be a shape corresponding to the intended secondary processing. For example, a tray having a shallow bottom, a tray with a flange (鍔) attached to the tray, a cylinder, or a deep drawn product (drawing ratio is 1 or more) can be used.
（２）第２の製造方法
最初の工程にて、結晶状態のポリフェニレンスルフィド（ＰＰＳ）を含む樹脂組成物からなるシートを得る。
この工程では、第１の製造方法と同じ方法によりシートを得た後、ＰＰＳの結晶化温度範囲内で保持して結晶状態にする。
(2) Second Production Method In the first step, a sheet made of a resin composition containing crystalline polyphenylene sulfide (PPS) is obtained.
In this step, after a sheet is obtained by the same method as the first manufacturing method, the sheet is held in the crystallization temperature range of PPS to be in a crystalline state.
次の工程にて、前工程で得られたシートをＰＰＳの融点（Tm）−４０℃以上から融点（Tm）−２０℃までの温度で予熱する。 In the next step, the sheet obtained in the previous step is preheated at a temperature from the melting point (Tm) of −40 ° C. or higher to the melting point (Tm) of −20 ° C. of PPS.
この予熱は、次工程で使用する成形機（真空成形機又は圧空成形機等）により行うことができる。予熱時間は、シートが上記温度範囲になるまでの時間である。 This preheating can be performed by a molding machine (such as a vacuum molding machine or a pressure molding machine) used in the next step. The preheating time is the time until the sheet reaches the above temperature range.
予熱温度が前記下限値以上であると、寸法精度良く中間成形品を得ることができ、予熱温度が前記上限値以下であると、成形時のドローダウンが防止できる。 When the preheating temperature is equal to or higher than the lower limit value, an intermediate molded product can be obtained with high dimensional accuracy, and when the preheating temperature is equal to or lower than the upper limit value, drawdown during molding can be prevented.
次の工程にて、予熱したシートを１０〜１５０℃に設定した金型内に入れて熱成形した後、さらに前記温度範囲で保持してＰＰＳの結晶化度が２０％以下である薄肉の中間成形品を得る。前記温度範囲は３０〜８０℃が好ましい。 In the next step, after the preheated sheet is put in a mold set at 10 to 150 ° C. and thermoformed, it is further held in the above temperature range, and the middle of the thin wall where the crystallinity of PPS is 20% or less Get a molded product. The temperature range is preferably 30 to 80 ° C.
金型温度が前記下限値以上であると、寸法精度良く薄肉の中間形品を得ることができ、金型温度が前記上限値以下であると、ＰＰＳが結晶化度２０％以下に結晶化される。 If the mold temperature is equal to or higher than the lower limit, a thin intermediate product can be obtained with good dimensional accuracy. If the mold temperature is equal to or lower than the upper limit, PPS is crystallized to a crystallinity of 20% or lower. The
薄肉の中間成形品の結晶化度は、２０％以下であり、０％（非晶状態）でもよい。 The crystallinity of the thin intermediate molded product is 20% or less, and may be 0% (amorphous state).
第２の製造方法で得られた薄肉の中間成形品の結晶化度、厚さ、形状は、第１の製造方法で得られたものと同じである。 The crystallinity, thickness, and shape of the thin intermediate molded product obtained by the second production method are the same as those obtained by the first production method.
本発明の製造方法により得られる中間成形品は、ＰＰＳ、繊維強化ＰＰＳもしくは他の樹脂又はそれらの成形体と一体化することにより、新たな用途の部材として使用するためのものである。前記一体化方法としては、金型内で溶融樹脂と接着させる方法、熱板溶着工法、超音波溶着工法、レーザー溶着工法、振動溶着工法、スピン溶着工法、熱線溶着工法、高周波誘電過熱溶着工法等が挙げられる。 The intermediate molded product obtained by the production method of the present invention is for use as a member for a new application by being integrated with PPS, fiber reinforced PPS or other resin, or a molded product thereof. Examples of the integration method include a method of adhering to a molten resin in a mold, a hot plate welding method, an ultrasonic welding method, a laser welding method, a vibration welding method, a spin welding method, a hot wire welding method, a high frequency dielectric superheating welding method, and the like. Is mentioned.
（１）温度測定
ＪＩＳ Ｋ−７１２１に準じた。ＰＰＳのガラス転移温度（Tg）、冷結晶化温度（Tcc）、融点（Tm）は、示差走査熱量測定計（DSC）を用い、２０℃／分の速度で昇温したときの熱量曲線の変曲点又は発熱ピークから求めた。
(1) Temperature measurement Conforms to JIS K-7121. The glass transition temperature (Tg), cold crystallization temperature (Tcc), and melting point (Tm) of PPS were measured by using a differential scanning calorimeter (DSC) and the change in the caloric curve when the temperature was raised at a rate of 20 ° C./min. Obtained from the inflection point or exothermic peak.
（２）成形性
真空成形時の成形性を下記の基準で評価した。
○：良好である（ドローダウンもなく、金型に対応した形状の成形品が得られた）。
△：成形品の形状が甘い（金型に対応した形状の成形品が得られない）か、或いは成形品が変形した。
×：ドローダウンが大きいか、或いはドローダウンが大きく、かつ成形品の形状も甘い（金型に対応した形状の成形品が得られない）。
(2) Formability The formability during vacuum forming was evaluated according to the following criteria.
○: Good (there was no drawdown and a molded product having a shape corresponding to the mold was obtained).
(Triangle | delta): The shape of a molded product is sweet (the molded product of the shape corresponding to a metal mold | die is not obtained), or the molded product deform | transformed.
X: The drawdown is large or the drawdown is large and the shape of the molded product is sweet (the molded product having a shape corresponding to the mold cannot be obtained).
（３）結晶化度
比重法により算出した。
(3) Crystallinity Calculated by the specific gravity method.
（４）接着性（他の樹脂との接着性）
縦１０ｃｍ、横１０ｃｍ、厚み３ｍｍのＰＰＳ板を３００℃に加熱し、溶融させた後に、成形品を載せ、更に１００ｇの錘を置き、２３℃の下で冷却固化させ、ＰＰＳ樹脂と成形品の接着強度を測定した。
◎：５０Ｎ以上
○：２０Ｎ以上、５０Ｎ未満
△：５Ｎ以上、２０Ｎ未満
×：５Ｎ未満
(4) Adhesiveness (adhesiveness with other resins)
A PPS plate with a length of 10 cm, width 10 cm, and thickness 3 mm is heated to 300 ° C. and melted, and then a molded product is placed on it, and a weight of 100 g is further placed and cooled and solidified at 23 ° C. The adhesive strength was measured.
◎: 50N or more ○: 20N or more, less than 50N Δ: 5N or more, less than 20N ×: less than 5N
（５）寸法精度
底面から７mmの深さ位置で４つの側面において各１点（計４点）の厚みを計測し、平均厚み（t1）を求めた。
同様に底面から１５mmの深さ位置で４つの側面において各１点（計４点）の厚みを計測し、平均厚み（t2）を求めた。
ｔ1／t2を算出して、その比が１．０に近いほど、寸法精度が良いことを意味する。
なお、成形品の寸法は、マイクロメータを用いて測定した。
(5) Dimensional accuracy The thickness of one point (4 points in total) was measured on each of the four side surfaces at a depth of 7 mm from the bottom, and the average thickness (t1) was determined.
Similarly, the thickness at one point (four points in total) was measured on each of the four side surfaces at a depth of 15 mm from the bottom surface, and the average thickness (t2) was determined.
When t1 / t2 is calculated, the closer the ratio is to 1.0, the better the dimensional accuracy.
The dimensions of the molded product were measured using a micrometer.
実施例１、２及び比較例１〜３
（シートの成形工程）
池貝社製のＶＳ40-25押出機（スクリュー径４０mm）にコートハンガーダイ（Ｔダイ：リップ300mm幅）を取り付けたものを用い、表１に示す（Ｔｇ、Ｔcc、Ｔｍ）のＰＰＳ（ポリプラスチックス（株）製）を溶融押出した。
押出後、外径２００mmの冷却ロール（ロール温度５０℃）にて冷却して、厚み０．８mmの非晶状態のシートを得た。結晶化度は１．７％であった。
Examples 1 and 2 and Comparative Examples 1 to 3
(Sheet forming process)
PPS (polyplastics) shown in Table 1 (Tg, Tcc, Tm) using a VS40-25 extruder (screw diameter: 40 mm) manufactured by Ikegai with a coat hanger die (T die: 300 mm wide). (Made by Co., Ltd.) was melt extruded.
After the extrusion, it was cooled with a cooling roll having an outer diameter of 200 mm (roll temperature: 50 ° C.) to obtain an amorphous sheet having a thickness of 0.8 mm. The crystallinity was 1.7%.
（予熱工程）
圧空真空成形機（ＦＫ−０４３１−１０（株）浅野研究所製）内にて、シート（250mm×250mm）が表１に示す温度になるまで予熱した。
(Preheating process)
In a compressed air vacuum forming machine (FK-0431-10 manufactured by Asano Laboratory), the sheet (250 mm × 250 mm) was preheated until the temperature shown in Table 1 was reached.
（成形工程）
真空成形用の金型として下記のものを用い、表１に示す金型温度及び保持時間で真空成形した。
(Molding process)
The following were used as vacuum molds, and vacuum molding was performed at the mold temperatures and holding times shown in Table 1.
金型：テーパー付き長方形開口トレイ
深さ：２ｃｍ
開口部：長さ７．１ｃｍ、幅５．４ｃｍ
底部：長さ６．７５ｃｍ、幅５．０５ｃｍ
Mold: Rectangular opening tray with taper Depth: 2cm
Opening: length 7.1cm, width 5.4cm
Bottom: length 6.75cm, width 5.05cm
実施例３及び比較例４〜６
（シートの成形工程）
冷却ロール温度を１５０℃とした以外、実施例１、２と同様にして０．８mmの結晶状態のシートにした。ＰＰＳはポリプラスチックス（株）の製品を用いた。結晶化度は、２５．５％であった。
Example 3 and Comparative Examples 4-6
(Sheet forming process)
A 0.8 mm crystalline sheet was obtained in the same manner as in Examples 1 and 2 except that the cooling roll temperature was 150 ° C. PPS used a product of Polyplastics Co., Ltd. The crystallinity was 25.5%.
（予熱工程）
圧空真空成形機（ＦＫ−０４３１−１０，（株）浅野研究所製）内にて、シート（250mm×250mm）が表１に示す温度になるまで予熱した。
(Preheating process)
In a compressed air vacuum forming machine (FK-0431-10, manufactured by Asano Laboratory Co., Ltd.), the sheet (250 mm × 250 mm) was preheated until the temperature shown in Table 1 was reached.
（成形工程）
予熱したシートを用い、実施例１、２と同様にして真空成形して、中間成形品を得た。
(Molding process)
Using the preheated sheet, vacuum forming was performed in the same manner as in Examples 1 and 2 to obtain an intermediate molded product.
Claims (2)
前記シートをＰＰＳのガラス転移温度（Tg）＋２０℃以上の温度から、冷結晶化温度（Tcc）＋１０℃以下の温度に予熱する工程、
予熱したシートを１０〜１５０℃に設定した金型内に入れて熱成形した後、さらに前記温度範囲で保持してＰＰＳの結晶化度が２０％以下である薄肉成形品を得る工程、
を有している薄肉の中間成形品の製造方法。 Obtaining a sheet comprising a resin composition containing amorphous polyphenylene sulfide (PPS);
Preheating the sheet from a glass transition temperature (Tg) of PPS + 20 ° C. or higher to a temperature of cold crystallization temperature (Tcc) + 10 ° C. or lower;
A step of obtaining a thin-walled molded article having a PPS crystallinity of 20% or less by holding the preheated sheet in a mold set at 10 to 150 ° C. and thermoforming, and further holding in the temperature range;
A method for producing a thin intermediate molded article having
前記シートをＰＰＳの融点（Tm）−４０℃以上から融点（Tm）−２０℃までの温度で予熱する工程、
予熱したシートを１０〜１５０℃に設定した金型内に入れて熱成形した後、さらに前記温度範囲で保持してＰＰＳの結晶化度が２０％以下である薄肉の中間成形品を得る工程、
を有している薄肉の中間成形品の製造方法。 Obtaining a sheet comprising a resin composition containing polyphenylene sulfide (PPS) in a crystalline state;
Preheating the sheet at a temperature from the melting point (Tm) of -40 ° C. or higher to the melting point (Tm) of -20 ° C .;
A step of obtaining a thin intermediate molded product having a PPS crystallinity of 20% or less by holding the preheated sheet in a mold set at 10 to 150 ° C. and thermoforming, and further holding in the above temperature range;
A method for producing a thin intermediate molded article having
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| JP2005169830A (en) * | 2003-12-11 | 2005-06-30 | Polyplastics Co | Molding method of heat radiating polyarylene sulfide resin composition and heat radiating molded product |
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|---|---|---|---|---|
| JPS63265618A (en) * | 1987-04-24 | 1988-11-02 | Kureha Chem Ind Co Ltd | Thermoformed polyarylene sulfide container and its preparation |
| JPH0569479A (en) * | 1991-09-12 | 1993-03-23 | Idemitsu Kosan Co Ltd | Sheet for thermoforming and fluorocarbon-resistant molded form |
| JPH05269830A (en) * | 1992-03-30 | 1993-10-19 | Polyplastics Co | Manufacture of thin form of crystalline polyarylene sulfide resin |
| JPH05269907A (en) * | 1992-03-30 | 1993-10-19 | Idemitsu Kosan Co Ltd | Styrenic resin laminate and molded object thereof |
| JP2005169830A (en) * | 2003-12-11 | 2005-06-30 | Polyplastics Co | Molding method of heat radiating polyarylene sulfide resin composition and heat radiating molded product |
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| JP2013018226A (en) * | 2011-07-13 | 2013-01-31 | Daicel Pack Systems Ltd | Method for manufacturing integral molding, and integral molding |
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