JP5771860B2 - 樹脂組成物の製造方法 - Google Patents
樹脂組成物の製造方法 Download PDFInfo
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- JP5771860B2 JP5771860B2 JP2011210454A JP2011210454A JP5771860B2 JP 5771860 B2 JP5771860 B2 JP 5771860B2 JP 2011210454 A JP2011210454 A JP 2011210454A JP 2011210454 A JP2011210454 A JP 2011210454A JP 5771860 B2 JP5771860 B2 JP 5771860B2
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
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- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Description
液晶ポリエステルは、成形時に分子鎖が流動方向に配向し易く、流動方向とその垂直方向とで成形収縮率や機械的性質に異方性が生じやすい。そのため、これを低減すべく、繊維状や板状などの種々の形状の充填材を配合して用いられている。
特許文献1には、(A)異方性溶融相を形成する液晶ポリエステル樹脂、及び液晶ポリエステルアミド樹脂から選ばれた少なくとも1種の液晶性樹脂100重量部に対して、(B)平均繊維径が3〜15μmのガラス繊維5〜300重量部を充填してなり、該組成物ペレット中の重量平均繊維長が0.02〜0.55mmの範囲にあって、且つ、繊維長が1mmを超えるガラス繊維の比率が該ガラス繊維の0〜15重量%、且つ、繊維長が0.1mm以下のガラス繊維の比率が該ガラス繊維の0〜50重量%であるガラス繊維強化液晶性樹脂組成物から得られたペレットを射出成形して、射出成形時の流動長さ、及び成形品の収縮率を求めているが、この技術は、ガラス繊維充填において、重量比や平均繊維長を制御する技術ではない。
また、予め平均繊維長を揃えた繊維状の充填材を配合することにより、液晶ポリエステル組成物中の充填材の平均繊維長を制御することも可能であるが、配合前に繊維状の充填材を繊維長で分級する必要があり、手間とコストがかかる。
本発明の樹脂組成物の製造方法において、繊維状充填材(B)が、ガラス繊維、カーボン繊維、バサルト繊維、アルミナ繊維からなる群から選択される無機充填材であることも好ましい。
図1は、本実施形態の樹脂組成物の製造方法で用いる押出機の一例を示す概略断面図である。以下、本実施形態の樹脂組成物の製造方法では、図1に示す押出機を用いて、樹脂(A)と繊維状充填材(B)とを溶融混練して樹脂組成物を製造することとして説明を行う。
シリンダー2には、最上流の位置(モーターボックス1側の位置)に、メインフィード口5が設けられ、メインフィード口5から下流側(押出方向後方;ダイ9側)に向けて、サイドフィード口7、第1ベント部4、第2ベント部6がこの順に設けられており、シリンダー2の下流側端部にはシリンダー2と連通するノズル穴9aを有する吐出ダイ9が設けられている。
また、第3混練部13にはニュートラルニーディングエレメントを用いるのが好ましい。
なお、スクリュー3が第3混練部13よりも押出方向後方(下流側)にさらに混練部を備える場合には、最下流に位置する混練部にニュートラルニーディングエレメントを用い、最下流以外の混練部にはニーディングディスクを位相角が0よりも大きく90度よりも小さくなるようにずらしながら重ねた構成のエレメントとニュートラルニーディングエレメントを用いることが好ましい。例えば、第1ベント部4と第2ベント部6にさらに第4混練部、第5混練部を備えている場合には、第1〜第4混練部のエレメントとして、ニーディングディスクを位相角が0よりも大きく90度よりも小さくなるようにずらしながら重ねた構成のエレメントとニュートラルニーディングエレメントを用い、第5混練部のエレメントとしてニュートラルニーディングエレメントを用いることが好ましい。
スクリュー3を構成するその他のエレメントには、溶融した樹脂組成物の全体的な搬送性を失わない限りは、どのようなスクリューエレメントを用いても良い。
本実施形態の樹脂組成物の製造方法に用いる樹脂(A)としては、液晶ポリエステル、ポリフェニレンサルファイド、ポリエーテルサルフォン、ポリアミド、ポリイミド等が挙げられ、特に液晶ポリエステルが好ましい。
(I)芳香族ヒドロキシカルボン酸と、芳香族ジカルボン酸と、芳香族ジオール、芳香族ヒドロキシアミン及び芳香族ジアミンからなる群から選ばれる少なくとも1種の化合物と、を重合(重縮合)させてなるもの、
(II)複数種の芳香族ヒドロキシカルボン酸を重合させてなるもの、
(III)芳香族ジカルボン酸と、芳香族ジオール、芳香族ヒドロキシアミン及び芳香族ジアミンからなる群から選ばれる少なくとも1種の化合物と、を重合させてなるもの、
(IV)ポリエチレンテレフタレート等のポリエステルと、芳香族ヒドロキシカルボン酸と、を重合させてなるもの、
が挙げられる。ここで、芳香族ヒドロキシカルボン酸、芳香族ジカルボン酸、芳香族ジオール、芳香族ヒドロキシアミン及び芳香族ジアミンは、それぞれ独立に、その一部又は全部に代えて、その重合可能な誘導体が用いられてもよい。
芳香族ヒドロキシカルボン酸、芳香族ジオール及び芳香族ヒドロキシアミンのようなヒドロキシル基を有する化合物の重合可能な誘導体の例としては、ヒドロキシル基をアシル化してアシルオキシル基に変換してなるもの(アシル化物)が挙げられる。
芳香族ヒドロキシアミン及び芳香族ジアミンのようなアミノ基を有する化合物の重合可能な誘導体の例としては、アミノ基をアシル化してアシルアミノ基に変換してなるもの(アシル化物)が挙げられる。
(2)−CO−Ar2−CO−
(3)−X−Ar3−Y−
前記アルキル基の例としては、メチル基、エチル基、n−プロピル基、イソプロピル基、n−ブチル基、イソブチル基、sec−ブチル基、tert−ブチル基、n−ペンチル基、n−ヘキシル基、n−ヘプチル基、2−エチルヘキシル基、n−オクチル基、n−ノニル基及びn−デシル基が挙げられ、その炭素数は、1〜10であることが好ましい。
前記アリール基の例としては、フェニル基、o−トリル基、m−トリル基、p−トリル基、1−ナフチル基及び2−ナフチル基が挙げられ、その炭素数は、6〜20であることが好ましい。
前記水素原子がこれらの基で置換されている場合、その数は、Ar1、Ar2又はAr3で表される前記基毎に、それぞれ独立に、2個以下であることが好ましく、1個以下であることがより好ましい。
繰返し単位(2)の含有量は、液晶ポリエステルを構成する全繰返し単位の合計量に対して、好ましくは35モル%以下、より好ましくは10〜35モル%、さらに好ましくは15〜30モル%、特に好ましくは17.5〜27.5モル%である。
繰返し単位(3)の含有量は、液晶ポリエステルを構成する全繰返し単位の合計量に対して、好ましくは35モル%以下、より好ましくは10〜35モル%、さらに好ましくは15〜30モル%、特に好ましくは17.5〜27.5モル%である。
繰返し単位(1)の含有量が多いほど、溶融流動性や耐熱性や強度・剛性が向上し易いが、あまり多いと、溶融温度や溶融粘度が高くなり易く、成形に必要な温度が高くなり易い。
本実施形態の製造方法に用いる繊維状充填材(B)は、繊維状無機充填材であっても、繊維状有機充填材であってもよい。
繊維状無機充填材の例としては、ガラス繊維;パン系炭素繊維、ピッチ系炭素繊維等の炭素繊維(カーボン繊維);シリカ繊維、アルミナ繊維、シリカアルミナ繊維等のセラミック繊維;ステンレス繊維等の金属繊維;及びバサルト繊維が挙げられる。また、チタン酸カリウムウイスカー、チタン酸バリウムウイスカー、ウォラストナイトウイスカー、ホウ酸アルミニウムウイスカー、窒化ケイ素ウイスカー、炭化ケイ素ウイスカー等のウイスカーも挙げられる。
繊維状有機充填材の例としては、ポリエステル繊維及びアラミド繊維が挙げられる。
成形加工時の装置に与える磨耗負荷や入手性を考慮すると、繊維状充填材(B)としては、ガラス繊維、カーボン繊維、バサルト繊維及びアルミナ繊維からなる群から選択される繊維状無機充填材が好ましく、中でもガラス繊維がさらに好ましい。
また、繊維状充填材(B)は、上記した充填材のうちの2種類以上の混合物であってもよい。また、繊維状充填材とそれ以外の充填材の混合物であってもよい。充填材の配合量は、液晶ポリエステル100質量部に対して、通常0〜100質量部である。
また、繊維状充填材(B)であるガラス繊維としては、エポキシ系、ウレタン系、アクリル系などの被覆あるいは集束剤で処理されたものであってもよい。
(i)押出機10のメインフィード口5から、樹脂(A)の一部量(X1)と、重量平均繊維長が1mm以上の繊維状充填材(B)の一部量(Y1)と、を供給し、
(ii)押出機10のサイドフィード口7から、前樹脂(A)の残量(X2)と、重量平均繊維長が1mm以上の繊維状充填材(B)の残量(Y2)と、を供給する。
ここで、樹脂(A)の押出機10への総供給量(P)=X1+X2(重量%)、繊維状充填材(B)の押出機10への総供給量(Q)=Y1+Y2(重量%)、樹脂(A)と繊維状充填材(B)の供給量の合計(P+Q)は100重量%である。
メインフィード口5に供給する繊維状充填材(B)の量(Y1)が前記範囲より多すぎると、押出機10への負荷が大きくなってしまう可能性がある。一方、メインフィード口5に供給する繊維状充填材(B)の量(Y1)が前記範囲より少なすぎると、得られる樹脂組成物中の繊維状充填材の平均繊維長が長くなり、該樹脂組成物を用いて成形を行う場合の樹脂組成物の流動性を阻害してしまう可能性がある。また、サイドフィード口7から供給するの樹脂(A)の量(X2)と繊維状充填材(B)の量(Y2)の比率が前記範囲を外れると、得られる樹脂組成物中の繊維状充填材の平均繊維長が長くなり、該樹脂組成物を用いて成形を行う場合の樹脂組成物の流動性を阻害してしまう可能性がある。
尚、メインフィード口5およびサイドフィード口7ともに、樹脂(A)と繊維状充填材(B)は、同時に供給することが望ましい。
得られた樹脂組成物中の繊維状充填材の重量平均繊維長は150〜350μm、好ましくは200〜300μm、さらに好ましくは200〜280μmである。また、得られた樹脂組成物中の繊維状充填材の数平均繊維長は100〜220μm、好ましくは100〜210μm、さらに好ましくは120〜200μmである。
樹脂組成物中の繊維状充填材の繊維長が上記範囲より短いと、該樹脂組成物を用いて得られる成形体の剛性が不足し、異方性が大きくなってしまう可能性がある。一方、樹脂組成物中の繊維状充填材の繊維長が上記範囲よりも長いと、該樹脂組成物を用いて成形体を成形する際に、樹脂組成物の流動性が阻害され成形性が悪化する可能性がある。また、樹脂組成物中の繊維状充填材の繊維長が上記範囲よりも長いと、該樹脂組成物を用いて得られる成形体の表面の概観が損なわれ、繊維状充填材の脱落やそれに由来する樹脂屑の発生などによる発塵性が悪化する可能性がある。
[繊維状充填材の繊維長の測定方法]
繊維状フィラーの重量平均繊維長と数平均繊維長は、樹脂組成物中にある繊維状充填材の外観形状で求めるものである。具体的に、これらの測定方法について説明する。
繊維状充填材の外観形状は、樹脂組成物のうち1.0gをるつぼに採取し、電気炉内にて600℃で4時間処理して灰化させ、その残渣をメタノールに分散させてスライドガラス上に展開させた状態で顕微鏡写真をとり、その写真から繊維状充填材の形状を直接的に読み取って、その平均値を算出して求められるものである。尚、平均値の算出にあたっては母数を400以上とする。各重量については、繊維状充填材の比重より各繊維長に対する重量を算出し、平均値の算出にあたっては用いた試料の全重量を用いる。
また、本発明の製造方法によれば、押出機10に供給する前の繊維状充填材を予め、所望の繊維長に分級する必要がないため、経済的に樹脂組成物中の繊維状充填材の繊維長が制御された樹脂組成物を製造できる。
攪拌装置、トルクメータ、窒素ガス導入管、温度計及び還流冷却器を備えた反応器に、p−ヒドロキシ安息香酸994.5g(7.2モル)、テレフタル酸299.0g(1.8モル)、イソフタル酸99.7g(0.6モル)、4,4’−ジヒドロキシビフェニル446.9g(2.4モル)、無水酢酸1347.6g(13.2モル)及び1−メチルイミダゾール0.194gを入れ、窒素ガス気流下、攪拌しながら、室温から145℃まで15分かけて昇温し、145℃で1時間還流させた。次いで、1−メチルイミダゾール0.194gを加え、副生酢酸及び未反応の無水酢酸を留去しながら、145℃から320℃まで3時間かけて昇温し、320℃で2時間保持した後、反応器から内容物を取り出し、室温まで冷却した。得られた固形物を、粉砕機で粉砕して、粉末状のプレポリマーを得た。このプレポリマーの流動開始温度は、261℃であった。次いで、このプレポリマーを、窒素ガス雰囲気下、室温から250℃まで1時間かけて昇温し、250℃から285℃まで5時間かけて昇温し、285℃で3時間保持することにより、固相重合させた後、冷却して、粉末状の液晶ポリエステルを得た。この液晶ポリエステルの流動開始温度は、327℃であった。このようにして得られた液晶ポリエステルをLCP1とした。
上記で得られたLCP1、ガラス繊維(日東紡績株式会社製CS−3J−260S)を、LCP1(X1、X2)及びガラス繊維(Y1、Y2)を表1に示す配分で、二軸押出機(東芝機械株式会社製TEM−41SS)を用いて溶融混練し、樹脂組成物を得た。
二軸押出機は、図1に示す構成の押出機に、第1ベント部に第4混練部が、第2ベント部に第5混練部が、それぞれ追加された構成のものを使用した。二軸押出機の混練部は、第1混練部から第4混練部までは5R及び5Nからなる構成で、第5混練部は5Nのみからなる構成とした。尚、Nは90度でずらして5枚重ね合わせたニュートラルニーディングセグメント、Rは30度ずつ右回転になるようにずらして5枚重ねたセグメントを表す。また、第2混練部から第5混練部までは剪断発熱を抑制するために240℃とした。それ以外は340℃とした。スクリュー径は41mmのものを使用し、第2ベント部は水流ポンプで真空度がゲージ圧で−0.09MPa(大気圧を0MPaとする)となるように保持した。スクリューは二軸同方向(右回転)のものを使用し、スクリュー回転数は700rpmとし、押出量は300kg/hrで行った。
得られた樹脂組成物中の繊維状充填材(ガラス繊維)の繊維長は以下の方法を用いて測定した。結果を表2に示した。
得られた樹脂組成物のうち1.0gをるつぼに採取し、電気炉内にて600℃で4時間処理して灰化させ、その残渣をメタノールに分散させてスライドガラス上に展開させた状態で顕微鏡写真をとり、その写真から繊維状充填材の形状を直接的に読み取って、その平均値を算出した。尚、平均値の算出にあたっては母数を400以上とした。各重量については、繊維状充填材の比重より各繊維長に対する重量を算出し、平均値の算出にあたっては用いた試料の全重量を用いた。
Claims (3)
- 押出機を用いて樹脂(A)と繊維状充填材(B)とを溶融混練して押し出す工程を含む樹脂組成物の製造方法であって、
シリンダーと、前記シリンダー内に配置されたスクリューと、前記シリンダーに設けられたメインフィード口と、前記シリンダーの前記メインフィード口より押出方向後方に設けられたサイドフィード口と、を備えた前記押出機を用い、
前記押出機のメインフィード口からの供給量(重量%)を、それぞれ、前記樹脂(A)の一部量(X1)と、前記繊維状充填材(B)の一部量(Y1)とし、
前記押出機の前記サイドフィード口からの供給量(重量%)を、それぞれ、前記樹脂(A)の残量(X2)と、前記繊維状充填材(B)の残量(Y2)とし(ただし、X1+X2+Y1+Y2=100重量%である)、
X1/X2=55/45〜70/30重量%比、Y1/Y2=75/25〜25/75重量%比、且つX2/Y2=90/10〜45/55重量%比となるように前記樹脂(A)および前記繊維状充填材(B)を前記押出機に供給することを特徴とする樹脂組成物の製造方法。 - 前記樹脂(A)が液晶ポリエステルであることを特徴とする請求項1に記載の樹脂組成物の製造方法。
- 繊維状充填材(B)が、ガラス繊維、カーボン繊維、バサルト繊維、アルミナ繊維からなる群から選択される無機充填材である請求項1又は2に記載の樹脂組成物の製造方法。
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CN100496930C (zh) * | 2004-04-15 | 2009-06-10 | 宝理塑料株式会社 | 控制纤维状填充剂长度的树脂组合物颗粒的制造方法 |
WO2006123824A1 (ja) * | 2005-05-18 | 2006-11-23 | Polyplastics Co., Ltd. | 繊維状充填剤高濃度配合樹脂組成物の製造方法及び樹脂組成物ペレット |
JP2008231368A (ja) * | 2007-03-23 | 2008-10-02 | Nippon Oil Corp | 光線反射率および強度に優れた液晶ポリエステル樹脂組成物 |
JPWO2009022516A1 (ja) * | 2007-08-10 | 2010-11-11 | 東亞合成株式会社 | 接着性樹脂組成物の製造方法及び樹脂フィルム並びに積層体 |
TW201119824A (en) * | 2009-06-30 | 2011-06-16 | Sumitomo Chemical Co | Method for producing resin composition, resin composition, reflection plate and light-emitting device |
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US9138915B2 (en) | 2015-09-22 |
US20130079454A1 (en) | 2013-03-28 |
CN103009595B (zh) | 2017-06-23 |
KR20130033970A (ko) | 2013-04-04 |
JP2013071281A (ja) | 2013-04-22 |
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