JP6935650B2 - 脂肪族ポリエステル樹脂組成物および成形体 - Google Patents
脂肪族ポリエステル樹脂組成物および成形体 Download PDFInfo
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- JP6935650B2 JP6935650B2 JP2017155278A JP2017155278A JP6935650B2 JP 6935650 B2 JP6935650 B2 JP 6935650B2 JP 2017155278 A JP2017155278 A JP 2017155278A JP 2017155278 A JP2017155278 A JP 2017155278A JP 6935650 B2 JP6935650 B2 JP 6935650B2
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Description
本発明は、ポリ(3−ヒドロキシアルカノエート)及び変性ナノセルロースを含有する脂肪族ポリエステル樹脂組成物に関する。以下では、ポリ(3−ヒドロキシアルカノエート)をP3HAと略して言及する。
本発明で用いられるP3HAとは、モノマー単位として3−ヒドロキシアルカン酸単位を含有するポリエステルであり、特に、式:[−CHR−CH2−CO−O−](式中、RはCnH2n+1で表される直鎖又は分岐鎖状のアルキル基を示し、nは1以上15以下の整数である。)で示される繰り返し単位を含むポリエステルが好ましい。該ポリエステルは単独重合体であってよいし、前記繰り返し単位を2種類以上含む共重合体であってもよい。このような共重合体は、単独重合体と比較して融点が低くなり得るために、溶融時の温度を低くすることができ、高温による変性ナノセルロースの変質を抑制できるため好ましい。
次に、本発明における変性ナノセルロースについて説明する。
植物の細胞壁の中では、幅4nm程のセルロースミクロフィブリル(シングルセルロースナノファイバー)が最小単位として存在しており、このセルロースミクロフィブリルが集まってセルロース繊維を構成し、植物の骨格を形成している。本発明でいう「ナノセルロース」とは、セルロース繊維を含む植物材料(例えば、木材パルプ等)を処理して、繊維をナノサイズレベルまで解きほぐして(解繊処理して)得られたセルロースナノファイバー(CNF)のことをいう。
本発明で用いる変性ナノセルロースのエステル置換度は、特に限定されず、成形物の強度や成形加工性の観点から適宜調節可能である。しかし、変性ナノセルロースをP3HA中で均一に分散させると共に、変性による効果が得やすい点から、0.05〜2.0程度が好ましく、0.1〜2.0程度がより好ましく、0.1〜0.8程度が更に好ましい。なお、上記エステル置換度とは、変性ナノセルロースにおけるセルロースを構成するグルコース骨格(グルコピラノース単位)に存在する3つの水酸基(2位、3位及び6位の水酸基)のうち、エステルで置換されたものの数(平均値)を示す。当該エステル置換度は、アルカリを添加し、エステル結合を加水分解することにより発生したカルボン酸量を滴定することにより算出できる。
CNFを変性して変性ナノセルロースを製造する方法は常法に従うことができる。特にジカルボン酸によってエステル化されている変性ナノセルロースを製造する方法について説明すると、CNFに対してジカルボン酸の無水物(無水ジカルボン酸)を反応させてモノエステル化させることで、式(I)で表される構造を有する変性ナノセルロースを製造することができる。無水ジカルボン酸を使用することで、触媒を用いなくてもモノエステル化を実施でき、CNFを効率よく変性できるため好ましい。
本発明の脂肪族ポリエステル樹脂組成物におけるP3HAの含有量は、特に限定されないが、50〜99重量%が好ましく、より好ましくは60〜98重量%、さらに好ましくは70〜95重量%である。
本発明の樹脂組成物には、本発明の効果を阻害しない範囲で公知の添加剤を添加することができる。具体的には、汎用プラスチックやポリ乳酸系樹脂等に対する増粘剤または結晶核剤を添加剤として配合することができる。そのような増粘剤または結晶核剤としては特に限定されないが、例えば、カーボンブラック、炭酸カルシウム、酸化ケイ素、ケイ酸塩、亜鉛華、ハイサイトクレー、カオリン、塩基性炭酸マグネシウム、マイカ、タルク、石英粉、ケイ藻土、ドロマイト粉、酸化チタン、酸化亜鉛、酸化アンチモン、硫酸バリウム、硫酸カルシウム、アルミナ、ケイ酸カルシウム、窒化ホウ素、塩化アンモニウム、架橋高分子ポリスチレン、ロジン系金属塩や、ガラス繊維、ウィスカー、炭素繊維等の無機繊維や、人毛、羊毛、竹繊維、パルプ繊維の有機繊維等が挙げられる。
本発明の樹脂組成物は、公知の方法で製造することができる。例えば、加熱溶融しつつP3HA、変性ナノセルロース、及び他の添加剤を混合して製造することができる。その際には、単軸押出機、2軸押出機、ニーダー、ギアポンプ、混練ロール、撹拌機を持つタンクなどを使用した機械的撹拌による混合や、流れの案内装置により分流と合流を繰り返す静止混合器を適用することができる。より具体的には、P3HA、変性ナノセルロース、及び他の添加剤を押出機、ロールミル、バンバリーミキサーなどにより溶融混練してペレット状とし、成形に供する方法、P3HAと高濃度の変性ナノセルロースを含有するマスターバッチを予め調製しておき、これとP3HAを所望の割合で溶融混練して成形に供する方法などが挙げられる。P3HAと変性ナノセルロースは混練機に同時に添加してもよいし、あるいは、P3HAを溶融させた後に変性ナノセルロースを添加して両成分の溶融混練を実施することもできる。
PHBHの重量平均分子量MwをGPC測定により求めた。GPC装置はLC−10Aシステム(島津製作所製)を使用し、カラムはGPCK−806M(昭和電工製)を使用し、カラム温度は40℃とした。対象物質3mgをクロロホルム2mlに溶解したものを、10μl注入して、ポリスチレン換算によりMwを求めた。
各実施例又は比較例では、P3HAとして、PHBH:ポリ(3−ヒドロキシブチレート−コ−3−ヒドロキシヘキサノエート)を使用した。このPHBHは、PHBH生産菌を培養した後、菌体から樹脂成分を回収して得たもので、HH率:PHBH中の3−ヒドロキシヘキサノエートのモル分率(mol%)は5.8mol%、Mwは55.6万である。なお、PHBH生産菌としては、Alcaligenes eutrophusに、Aeromonas caviae由来のPHA合成酵素遺伝子を導入したAlcaligenes eutrophus AC32(J.Bacteriol.,179,4821(1997))を使用した。
各実施例では、変性ナノセルロースとして、ヘキサデセニル基(炭素数が16のアルケニル基)を有する無水コハク酸でナノセルロースをモノエステル化した変性ナノセルロースを使用した。なお、当該変性ナノセルロースは、特許第5496435号公報に開示された製造方法により製造した。
PHBH100重量部に対してベヘン酸アミド(BA)0.5重量部、エルカ酸アミド(EA)0.5重量部をドライブレンドして粉体の混合物(以下、「粉体混合物」と称する場合がある)を得た。
まず、粉体混合物66重量部と30%粉MB33重量部を押出機外で混合した後、押出機に供給してペレット化した後、射出成形を行なって大きさが10mm×80mm×4mmの短冊状の試験片を得た。以下では、これを、一度練りの試験片という。
粉体混合物を押出機に供給してペレット化した後、射出成形を行なって大きさが10mm×80mm×4mmの短冊状の試験片を得た。射出成形時の金型温度を35℃に変更した以外の製造条件は実施例1と同様である。該試験片はセルロース系材料を含有していない。
変性ナノセルロースの代わりに、未変性ナノセルロース(セリッシュKY100G、ダイセルファインケム(株)製)を使用したこと以外は実施例1と同様にして、各試験片を得た。ただし、射出成形時の金型温度を35℃に変更した。各試験片は、樹脂組成物全体に対して10重量%を占める量でナノセルロースを含む。
変性ナノセルロースの代わりに、未変性の漂白パルプを使用したこと以外は実施例1と同様にして、各試験片を得た。ただし、射出成形時の金型温度を35℃に変更した。各試験片は、樹脂組成物全体に対して10重量%を占める量で漂白パルプを含む。
アニールを実施していない実施例1の三度練りの試験片を150℃の条件で加熱プレスして、光学顕微鏡によりクロスニコル下で偏光観察を行なった。撮影した顕微鏡写真を図1に示す。
万能試験機((株)島津製作所製、AG5000E型)を用いて速度10mm/min,支点間距離=64mmで三点曲げ試験を行い、各試験片の曲げ弾性率と曲げ強度を測定した。結果を表1及び2に示す。
日立ハイテクサイエンス社製DSC6220を用いて、各試験片の温度を23℃から200℃まで上昇させた後、23℃まで降下させることにより、結晶化ピーク温度(Tch)を測定した。また、結晶化度は、Macromolecules,28(1995),pp.4822−4828(「参考文献」と称する)に記載のP(3HB−co−5% 3HH)の結晶化度(参考文献のTable2,no2に記載)と、結晶化ピーク面積(ΔHm、参考文献のTable3,no2に記載)の値を元に、各試験片の結晶化ピーク面積(ΔHm)に係数0.609(非特許文献1から算出した係数)を乗じ、樹脂成分の含有率で除した下記の計算式1により算出した。結果を表3に示す。
結晶化度(%)=ΔHm x 0.609/(樹脂成分含有率)
<ペレットの調製>
上述した粉体混合物と30%粉MBを、樹脂組成物全体に対する変性ナノセルロース濃度が0.25重量%、5.0重量%、又は10重量%になるような割合で押出機外で混合した。次に、東芝機械社製の2軸押出機TEM26SSを用いて、各濃度の混合物をシリンダー温度120〜140℃で溶融混練し、φ4mm、3穴のストランドから溶融樹脂を吐出させ、設定60℃の温水で満たされた1.5m長の温浴槽内を通過させて結晶化、固化して、ペレタイザーにてペレット状にカットした。最後にカットしたペレットを60℃で一昼夜乾燥して固化試験に使用した。
固化試験は次のように実施した。DSM社製小型混練機XPloreシリーズMC5を用いて、変性ナノセルロース濃度が異なる各ペレットを設定温度170℃、スクリュー回転数100rpm、混練時間3分で溶融混練した後、溶融した樹脂を約55℃の温浴に投入し、溶融樹脂が固化するのに要した時間を測定した。結晶化が早いほど固化時間が短くなるので、固化試験では数字が小さいほど固化特性が優れていることを意味する。固化特性に優れていることは、成形加工の際に迅速に固化させることができ、成形体を優れた生産性で製造できる(即ち、成形加工性に優れる)ことを意味する。同じ手順で固化時間の測定を3回行い、その平均値を表4に示した。
Claims (5)
- ポリ(3−ヒドロキシアルカノエート)及び変性ナノセルロースを含有し、
前記変性ナノセルロースは、セルロースが有する水酸基がアルキル基又はアルケニル基を有するコハク酸によってエステル化されている変性ナノセルロースであり、
前記ポリ(3−ヒドロキシアルカノエート)は、モノマー単位として3−ヒドロキシアルカン酸単位を2種類以上含有する共重合体、及び、モノマー単位として3−ヒドロキシアルカン酸単位と3−ヒドロキシアルカン酸単位以外のヒドロキシアルカン酸単位とを含有する共重合体からなる群より選択される少なくとも1種の共重合体を含み、
前記ポリ(3−ヒドロキシアルカノエート)の重量平均分子量が、50,000〜3,000,000である、脂肪族ポリエステル樹脂組成物。 - ポリ(3−ヒドロキシアルカノエート)が、式:[−CHR−CH2−CO−O−](式中、Rは、炭素数1〜15の直鎖又は分岐鎖状のアルキル基を示す)で示される繰り返し単位を含む、請求項1に記載の脂肪族ポリエステル樹脂組成物。
- ポリ(3−ヒドロキシアルカノエート)が、ポリ(3−ヒドロキシブチレート−コ−3−ヒドロキシバレレート)、ポリ(3−ヒドロキシブチレート−コ−3−ヒドロキシバレレート−コ−3−ヒドロキシヘキサノエート)、ポリ(3−ヒドロキシブチレート−コ−3−ヒドロキシヘキサノエート)、及び、ポリ(3−ヒドロキシブチレート−コ−4−ヒドロキシブチレート)からなる群より選択される少なくとも1種である、請求項1に記載の脂肪族ポリエステル樹脂組成物。
- 変性ナノセルロースの含有量が、ポリ(3−ヒドロキシアルカノエート)100重量部に対して1〜100重量部である、請求項1〜3のいずれか1項に記載の脂肪族ポリエステル樹脂組成物。
- 請求項1〜4のいずれか1項に記載の脂肪族ポリエステル樹脂組成物を成形してなる成形体。
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