Morphologies and Mechanical Properties of the Nanocomposites of Poly(butylene succinate-co-lactate) and the Organo-modified Montmorillonites Treated w

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1 Morphologies and Mechanical Properties of the Nanocomposites of Poly(butylene succinate-co-lactate) and the Organo-modified Montmorillonites Treated with Alkyltrimethoxysilanes SOMEYA Yoshihiro, SHIBATA Mitsuhiro, MINAKUCHI Ryo, MORIYA Takashi, TAKEI Toshio, and MORITA Tsuyoshi The montmorillonite treated with hexyltrimethoxysilane (HTMS) or octadecyltrimethoxysilane (OTMS) was further ion-exchanged by N-lauryldiethanolamine (LEA) hydrochloride. The composites of biodegradable poly(butylene succinate-co-lactate) (PBSL) and the obtained LEAmodified montmorillonites treated with HTMS or OTMS (HTMS-LEA-M or OTMS-LEA-M) were prepared by polymer melt intercalation method. Although the obtained composites had little difference in the quantity of intercalated polymer as compared with PBSL/LEA-modified montmorillonite as a result of X-ray diffraction analysis, transmission electron microscopy studies of the PBSL composites revealed that the extent of clay dispersion is certainly improved. Especially the PBSL/OTMS-LEA-M composites had a very fine and homogeneous dispersion of clay. The storage modulus at the rubbery state and tan peak temperature by dynamic viscoelastic measurement of the composites increased by use of HTMS-LEA-M or OTMS-LEA-M. The use of the alkyltrimethoxysilane-treated clay was also effective for the increase of tensile modulus. Especially, the PBSL/OTMS-LEA-M nanocomposites with inorganic content 5 wt% and 10 wt% had 2 and 3.5 times higher tensile moduli than the control PBSL, respectively. 1 DIC Technical Review No.13 /

2 DIC Technical Review No.13 / 2007

3 Fig. 3 TGA curves of LEA-M, HTMS-LEA-M, and OTMS- LEA-M. Fig. 1 IR spectra of (a)otms-m, (b)htms-m, (c)mmt, (d)otms-lea-m, (e)htms-lea-m, and (f)lea-m. Fig. 2 TGA curves of MMT, HTMS-M, and OTMS-M DIC Technical Review No.13 /

4 報 文 Fig. 4 XRD patterns of clays and the PBSL/clay composites. る赤外線吸収ピークが強く観測されておりシランカッ できないが シランカップリング処理の有無がイオ プリング処理の有無による違いは確認できなかった ン交換率に与える影響は小さいと考えられる Fig. 1 (d)-(f) いずれのクレイもLEA塩酸塩により 同程度にイオン交換されており シランカップリン グ処理により導入されたアルキル基はLEAによる有機 3.2 各種クレイの構造とPBSL中でのクレイの分 散性 化処理によるものよりも非常に少ないことを示唆し クレイ単体およびPBSL/クレイ複合材料のXRDチャ ている Fig. 3にLEA-M HTMS-LEA-MおよびOTMS- ートをFig. 4に示した 珪酸塩層の[001]面の反射によ LEA-MのTGA曲線を示した いずれのLEA処理クレ るXRDピークの2θ値とBraggの式から算出した珪酸 イもTGA曲線では200から500 に2段階のプロトン化 塩層の層間距離をTable 1にまとめて示した クレイ LEA成分の分解が確認され その重量減少はLEA-M 単体の層間距離をd 1 PBSL/クレイ複合材料の層間距 HTMS-LEA-M OTMS-LEA-Mでそれぞれ 離を d 2 両者の層間距離の差 d 2 d 1 をΔ d で表し 21.7 であった それらの値とMMTの理論イオン交 てある クレイ単体の d 1 について MMTが1.26 nm 換容量 eq/100 g から求めたイオン交換率は シランカップリング処理を行ったHTMS-MとOTMS-M それぞれ となった ただし この が1.19 nmと0.97 nmであり アルキル基含量が増える イオン交換率の計算においてクレイ層間水とシラン につれて数値的には少し低下した アルキル基導入 カップリング処理によるアルキル基の分解による重 による直接的な影響ではないが クレイ端面の疎水 量減少分は無視されているので厳密な数値の比較は 化により層間水が減少してd 1が低下しているものと考 10 DIC Technical Review No.13 / 2007

5 Table 1 Interlayer Spacing of Clays and PBSL/Clay Composites as Determined by XRD Analysis Fig. 5 TEM images of PBSL/clay composites with inorganic content 3 wt%: (a), (b) PBSL/LEA-M; (c), (d) PBSL/HTMS-LEA-M; and (e), (f) PBSL/OTMS-LEA-M. DIC Technical Review No.13 /

6 報 文 Fig. 6 Dynamic viscoelastic properties of PBSL/clay composites: (a) PBSL/clay composites with inorganic content 3 wt%, (b) PBSL/HTMS-LEA-M, and (c) PBSL/OTMS-LEA-M composites. えられる 一方 嵩高いアンモニウム塩が層間に挿 Clay Product Inc., Cloisite 25A を グリシドキシプ 入されたLEA-Mはd 1が1.81 nmとmmtに比べて層間が ルピル トリメトキシシラン処理した場合 層間距 0.55 nm拡大していた さらにシランカップリング処 離がほとんど変化しないことが報告されている 25,26) 理したHTMS-LEA-MおよびOTMS-LEA-Mのd 1はLEA- 本研究の場合も含めて 珪酸塩層の端面に嵩高い置 Mとほぼ同等であり シランカップリング処理による 換基が結合しても層間距離には直接的には影響しな 層間距離への影響は見られなかった いずれのクレ いようである イもLEAにより疎水化されていることから層間水含量 MMT HTMS-MおよびOTMS-Mを使用した場合 にあまり差がないためであると考えられる 実際に PBSL/クレイ複合材料の層間距離はクレイ単体と比べ 嵩高いアルキルアンモニウム処理MMT Southern てほとんど拡大しておらず 層間へのポリマーの挿 12 DIC Technical Review No.13 / 2007

7 3.3 Fig. 7 Tensile properties vs. inorganic content for PBSL/clay composites. DIC Technical Review No.13 /

8 DIC Technical Review No.13 / 2007

9 SOMEYA Yoshihiro SHIBATA Mitsuhiro MINAKUCHI Ryo MORIYA Takashi MORITA Tsuyoshi TAKEI Toshio DIC Technical Review No.13 /

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