JP2016079212A - 加熱圧縮成形用成形材料及びその成形品 - Google Patents
加熱圧縮成形用成形材料及びその成形品 Download PDFInfo
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- JP2016079212A JP2016079212A JP2014208985A JP2014208985A JP2016079212A JP 2016079212 A JP2016079212 A JP 2016079212A JP 2014208985 A JP2014208985 A JP 2014208985A JP 2014208985 A JP2014208985 A JP 2014208985A JP 2016079212 A JP2016079212 A JP 2016079212A
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- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
【解決手段】熱硬化性樹脂(a1)、ラジカル重合性希釈剤(a2)及び熱可塑性樹脂(a3)を必須成分とする樹脂成分(A)と、無機充填材(B)と、フッ素化アルキル基を有する(メタ)アクリレート化合物(c1)及びアルキル(メタ)アクリレート化合物(c2)を必須成分とする重合性モノマーを共重合して得られるフッ素系共重合体(C)と、ノニオン系界面活性剤(D)とを含有するコンパウンドを、ガラス繊維に含浸して得られることを特徴とする加熱圧縮成形用成形材料を用いる。
【選択図】なし
Description
測定装置:東ソー株式会社製「HLC−8220 GPC」、
カラム:東ソー株式会社製ガードカラム「HHR−H」(6.0mmI.D.×4cm)
+東ソー株式会社製「TSK−GEL GMHHR−N」(7.8mmI.D.×30cm)
+東ソー株式会社製「TSK−GEL GMHHR−N」(7.8mmI.D.×30cm)
+東ソー株式会社製「TSK−GEL GMHHR−N」(7.8mmI.D.×30cm)
+東ソー株式会社製「TSK−GEL GMHHR−N」(7.8mmI.D.×30cm)
検出器:ELSD(オルテックジャパン株式会社製「ELSD2000」)
データ処理:東ソー株式会社製「GPC−8020モデルIIデータ解析バージョン4.30」
測定条件:カラム温度 40℃
展開溶媒 テトラヒドロフラン(THF)
流速 1.0ml/分
試料:樹脂固形分換算で1.0質量%のテトラヒドロフラン溶液をマイクロフィルターでろ過したもの(5μl)。
標準試料:前記「GPC−8020モデルIIデータ解析バージョン4.30」の測定マニュアルに準拠して、分子量が既知の下記の単分散ポリスチレンを用いた。
東ソー株式会社製「A−500」
東ソー株式会社製「A−1000」
東ソー株式会社製「A−2500」
東ソー株式会社製「A−5000」
東ソー株式会社製「F−1」
東ソー株式会社製「F−2」
東ソー株式会社製「F−4」
東ソー株式会社製「F−10」
東ソー株式会社製「F−20」
東ソー株式会社製「F−40」
東ソー株式会社製「F−80」
東ソー株式会社製「F−128」
東ソー株式会社製「F−288」
東ソー株式会社製「F−550」
温度計、攪拌機、不活性ガス導入口および還流冷却器を備えたガラスフラスコに、無水マレイン酸3モル、イソフタル酸1モル、ネオペンチルグリコール2モル及びプロピレングリール2モルを仕込み、窒素気流中、攪拌しながら、205℃にて10時間、脱水縮合反応した。次いで、スチレンを添加し、不飽和ポリエステル樹脂(a1−1)の60質量%スチレン溶液を得た。この不飽和ポリエステル樹脂(a1−1)の酸価は14mgKOH/gであった。
温度計、撹拌機、不活性ガス導入口、還流冷却器および滴下装置を備えたガラスフラスコに、トルエンを200質量部入れ、窒素気流中、攪拌しながら105℃に昇温した。次いで、3,3,4,4,5,5,6,6,7,7,8,8,8−トリデカフルオロオクチルアクリレート55質量部及びステアリルアクリレート45質量部をトルエン125質量部に溶解したモノマー溶液と、t−ブチルペルオキシ−2−エチルヘキサノエート8質量部をトルエン20質量部に溶解したラジカル重合開始剤溶液との2種類の滴下液をそれぞれ別々の滴下装置にセットし、フラスコ内を105℃に保ちながら同時に2時間かけて滴下した。滴下終了後、105℃で13時間攪拌した後、減圧下で溶媒を留去することにより、フッ素系共重合体(C−1)を得た。このフッ素系共重合体(C−1)のフッ素原子の含有率は32質量%であった。
温度計、撹拌機、不活性ガス導入口、還流冷却器および滴下装置を備えたガラスフラスコに、トルエンを200質量部入れ、窒素気流中、攪拌しながら105℃に昇温した。次いで、下記式(1)で表されるフルオロアルキルエーテル基を有するアクリレート30質量部および下記式(2)で表される平均繰り返し単位数6のポリオキシアルキレン鎖を有するポリプロピレングリコールモノメタクリレート70質量部をトルエン125質量部に溶解したモノマー溶液と、t−ブチルペルオキシ−2−エチルヘキサノエート8質量部をトルエン20質量部に溶解したラジカル重合開始剤溶液との2種類の滴下液をそれぞれ別々の滴下装置にセットし、フラスコ内を105℃に保ちながら同時に2時間かけて滴下した。滴下終了後、105℃で13時間攪拌した後、減圧下で溶媒を留去することにより、比較用フッ素系共重合体(RC−1)を得た。この比較用フッ素系共重合体(RC−1)のフッ素原子の含有率は8.1質量%であった。
合成例1で得られた不飽和ポリエステル樹脂(a1−1)の60質量%スチレン溶液80質量部、ポリスチレンの35質量%スチレン溶液(ディーエイチ・マテリアル株式会社製「PS−954」)20質量部、炭酸カルシウム(平均粒子径3μm)160質量部、合成例2で得られたフッ素系共重合体(C−1)1質量部、デカグリセリンオレイン酸エステル(阪本薬品工業株式会社製「DOA−7S」)5質量部、重合開始剤(化薬アクゾ株式会社製「カヤカルボンBIC−75」)1質量部、酸化マグネシウム1質量部、ステアリン酸亜鉛3部をディゾルバーにより混合し、コンパウンド(1)271質量部を得た。
製造例1で用いたフッ素系共重合体(C−1)及びデカグリセリンオレイン酸エステルを用いなかった以外は、製造例1と同様に操作することにより、比較用コンパウンド(R1)265質量部を得た。
製造例1で用いたデカグリセリンオレイン酸エステルを用いなかった以外は、製造例1と同様に操作することにより、比較用コンパウンド(R2)266質量部を得た。
製造例1で用いたフッ素系共重合体(C−1)を用いなかった以外は、製造例1と同様に操作することにより、比較用コンパウンド(R3)270質量部を得た。
製造例1で用いたデカグリセリンオレイン酸エステルを用いず、且つ、フッ素系共重合体(C−1)1質量部の代わりに、合成例3で得られた比較用フッ素系共重合体(RC−1)5質量部を用いた以外は、製造例1と同様に操作することにより、比較用コンパウンド(R4)270質量部を得た。
製造例1で用いたフッ素系共重合体(C−1)1質量部の代わりに、合成例3で得られた比較用フッ素系共重合体(RC−1)5質量部を用いた以外は、製造例1と同様に操作することにより、比較用コンパウンド(R5)275質量部を得た。
製造例1で得られたコンパウンド(1)271質量部を上下に設置された2枚のポリプロピレン製キャリアフィルム上に均一な厚さになるように塗布し、25.4mmにカットしたガラス繊維(日東紡績株式会社製「PB−549」)93質量部を前記上下に設置されたキャリアフィルム上の樹脂組成物の間に挟み込み、全体を含浸ロールの間に通して圧力を加えてコンパウンド(1)をガラス繊維に含浸させた後、45℃で24時間養生し、ガラス繊維含有率が25.5質量%の加熱圧縮成形用成形材料(1)を得た。また、加熱圧縮成形用成形材料(1)中のフッ素原子含有率は、0.09質量%であった。
上記で得られた加熱圧縮成形用成形材料(1)650gを300×300mmの金型を用いて加熱圧縮成形し、厚さ4mmの平板状の成形品(1)を得た。加熱圧縮成形条件は、金型温度が上型145℃、下型130℃とし、キープ時間6分間、印加圧力10MPaとした。尚、得られた成形品(1)の上型側を評価面とした。
上記で得られた成形品(1)について、協和界面科学株式会社製の全自動接触角計CA−V型を用いて、JIS K6768に準拠し、常温下、蒸留水を用いた液滴法で水接触角測定し、下記の基準により、成形品の撥水性を評価した。
○:接触角が100度以上
△:接触角が95度以上100度未満
×:接触角が95度未満
上記で得られた成形品(1)について、上記の[成形品の水接触角測定]で用いた蒸留水の代わりにオレイン酸液を用いた以外は同様の手法を用いてオレイン酸接触角を測定し、下記の基準により、成形品の撥油性を評価した。
○:接触角が50度以上
△:接触角が45度以上50度未満
×:接触角が45度未満
実施例1で用いたコンパウンド(1)271質量部を、製造例2で得られた比較用コンパウンド(R1)265質量部に変更した以外は、実施例1と同様に操作することにより、ガラス繊維含有率26.0質量%の比較用加熱圧縮成形用成形材料(R1)を得た。この比較用加熱圧縮成形用成形材料(R1)のフッ素原子含有率は0質量%であった。
実施例1で用いたコンパウンド(1)を、比較用コンパウンド(R2)〜(R5)に変更した以外は、実施例1と同様に操作することにより、比較用加熱圧縮成形用成形材料(R2)〜(R5)を得た。それぞれのガラス繊維含有率は、(R2)が25.9質量%、(R3)が25.6質量%、(R4)が25.6質量%、(R5)が25.3質量%であった。また、それぞれのフッ素原子含有率は、(R2)が0.09質量%、(R3)が0質量%、(R4)が0.11%、(R5)が0.11質量%であった。
実施例1で用いた加熱圧縮成形用成形材料(1)を、上記で得られた比較用加熱圧縮成形用成形材料(R1)〜(R5)に変更した以外は、実施例1と同様に操作することにより、比較用成形品(R1)〜(R5)を作製して、成形品の水接触角及びオレイン酸接触角を測定し、撥水性及び撥油性を評価した。
Claims (7)
- 熱硬化性樹脂(a1)、ラジカル重合性希釈剤(a2)及び熱可塑性樹脂(a3)を必須成分とする樹脂成分(A)と、無機充填材(B)と、フッ素化アルキル基を有する(メタ)アクリレート化合物(c1)及びアルキル(メタ)アクリレート化合物(c2)を必須成分とする重合性モノマーを共重合して得られるフッ素系共重合体(C)と、ノニオン系界面活性剤(D)とを含有するコンパウンドを、ガラス繊維に含浸して得られることを特徴とする加熱圧縮成形用成形材料。
- 前記コンパウンドが、前記樹脂成分(A)100質量部に対して、前記無機充填材(B)を30〜350質量部、前記フッ素系共重合体(C)を0.5〜5質量部、前記ノニオン系界面活性剤(D)を1〜10質量部含有するものである請求項1記載の
加熱圧縮成形用成形材料。 - 前記熱硬化性樹脂(a1)が不飽和ポリエステル樹脂である請求項1又は2記載の加熱圧縮成形用成形材料。
- 前記フッ素系共重合体(C)のフッ素化アルキル基が、パーフルオロアルキル基である請求項1〜3のいずれか1項記載の加熱圧縮成形用成形材料。
- 前記ノニオン系界面活性剤(D)が、(ポリ)グリセリン脂肪酸エステルである請求項1〜4のいずれか1項記載の加熱圧縮成形用成形材料。
- 前記加熱圧縮成形用成形材料が、シートモールディングコンパウンド(SMC)又はバルクモールディングコンパウンド(BMC)である請求項1〜5のいずれか1項記載の加熱圧縮成形用成形材料。
- 請求項1〜6のいずれか1項記載の加熱圧縮成形用成形材料を成形して得られたものであることを特徴とする成形品。
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Citations (5)
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JPS52996A (en) * | 1975-06-24 | 1977-01-06 | Hitachi Chem Co Ltd | Resin composition |
JPH06271839A (ja) * | 1993-03-17 | 1994-09-27 | Asahi Glass Co Ltd | 水分散型フッ素系撥水撥油剤組成物 |
JPH0711092A (ja) * | 1993-06-29 | 1995-01-13 | Japan Synthetic Rubber Co Ltd | 熱硬化性樹脂組成物 |
JPH0770451A (ja) * | 1993-06-30 | 1995-03-14 | Sumitomo Chem Co Ltd | 熱硬化性樹脂組成物、熱硬化物およびその製造方法 |
WO2005047417A1 (ja) * | 2003-11-13 | 2005-05-26 | Daikin Industries, Ltd. | 撥水撥油剤水性分散液 |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS52996A (en) * | 1975-06-24 | 1977-01-06 | Hitachi Chem Co Ltd | Resin composition |
JPH06271839A (ja) * | 1993-03-17 | 1994-09-27 | Asahi Glass Co Ltd | 水分散型フッ素系撥水撥油剤組成物 |
JPH0711092A (ja) * | 1993-06-29 | 1995-01-13 | Japan Synthetic Rubber Co Ltd | 熱硬化性樹脂組成物 |
JPH0770451A (ja) * | 1993-06-30 | 1995-03-14 | Sumitomo Chem Co Ltd | 熱硬化性樹脂組成物、熱硬化物およびその製造方法 |
WO2005047417A1 (ja) * | 2003-11-13 | 2005-05-26 | Daikin Industries, Ltd. | 撥水撥油剤水性分散液 |
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R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |