JP2011527363A - 半結晶ポリマーの熱処理方法 - Google Patents
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Abstract
Description
a)粒状材料を流通式設備に供給し、
b)その粒状材料を加熱ゾーン中で加熱しながら、粒状材料をその加熱ゾーンの中を通過させ、
c)任意選択で、さらに流通式設備中の粒状材料を搬送しながら、その粒状材料を高温に保ちかつ/またはその粒状材料を冷却し、
d)その流通式設備から粒状材料を吐出する
ステップを含む。
−各加熱ゾーンが、一連の加熱プレートからなる接触型ヒーターを備え、
−粒状材料がこの流通式設備に供給され、
−この粒状材料が、本質的に移動充填層として加熱ゾーン中、または複数加熱ゾーン中に搬送され、
−この粒状材料が流通式設備から吐出され、
−粒状材料は、少なくとも70%がその接触型ヒーターから来る、または2つ以上の接触型ヒーターの場合はそれら接触型ヒーターから来るエネルギー入力によって加熱され、
−任意選択で不活性ガスの流れが加熱ゾーンの1つまたは複数に加えられ、もしあれば各加熱ゾーン中の不活性ガス流量が、多くとも2の質量比G/M(Gは単位kg/時の不活性ガスの流量であり、Mは単位kg/時のその特定の材料の流量である)であるという条件を満たす。
試験は、その上端に粒状材料の供給手段とその下端に吐出し手段とを有し、かつ一方向に狭くなる長方形の吐出しゾーンを含む長方形断面の細長い垂直に位置決めされた容器として本質的に特徴づけられる装置中で行った。加熱ゾーンは、調整可能な間隔を有する加熱プレートを含む。プレートは高さ600mm、幅300mmである。プレートは、油で加熱され、Lauda熱媒油ユニットにより制御された二重壁プレートである。
ガラス充填ポリエステルの目詰りおよびブリッジング挙動を測定するために幾つかの実験を行った。この実験は、流通ユニットを造粒された材料で満たし、続いてこの流通ユニットに追加の造粒された材料を供給し、同時に造粒された材料を移動固定層として流通ユニットを通過させることによって加熱されたプレートに渡すことにより行った。一般にこの生成物中のポリマーは、メタクレゾールに25℃で溶かした1%濃度において測定される1.45の相対粘度を有した。グラニュールは、設備に室温でその上部から入れた。その際にこの工程、すなわち結晶化ステップの最も決定的に重要な意味をもつ相を調べた。このために材料を目視検査した。グラニュールの結晶化は、色のわずかな変化によって目で見ることができた。さらに実験を、その生成物の流動性を適時に調べるためにプレキシグラスフロントプレートを通して視覚的に続けた。
結晶化ステップの後、生成物は平板熱交換器を備えた後縮合部分へ重力によってさらに流れ下り、そこで生成物は平板熱交換器のプレート全体にわたってむらのない分布を達成した。加熱プレートに沿って下へ移動しながら、生成物は220℃の設定温度を有するプレートに接触することによって加熱され、ゆっくり後縮合温度に到達する。これらプレートの長さは、熱交換器を離れる生成物が、プレートのうちの1枚と接触している材料と、それらプレートのちょうど中間にある材料との間で1℃以下の温度差を有するような長さであった。窒素ガスは、生成物に対する向流として加熱ゾーンを通って流れた。加熱ゾーンの後、生成物は、窒素が向流として流れる状態で反応ゾーンを通って下方へゆっくり移動し、それによって揮発性反応生成物が除去された。反応ゾーンを離れた後、生成物はひと揃いの冷却プレートを含む冷却ゾーンに入った。そこで生成物は、冷却プレートによる熱交換によって50℃まで冷却された。この冷却ゾーンの後、生成物は一方向に細くなる円錐体および吐出し回転弁を介して吐出されて緩衝容器に入る。
Claims (10)
- 1または複数の加熱ステップを含む、固体の状態において熱可塑性半結晶ポリマーを含む粒状熱可塑性材料を熱処理するための連続法であって、
−前記方法が1または複数の加熱ゾーンを含む流通式設備中で行われ、
−各加熱ゾーンが一連の加熱プレートからなる接触型ヒーターを備え、
−前記粒状材料が前記流通式設備に供給され、
−前記粒状材料が、本質的に移動充填層として前記加熱ゾーン中または前記複数の加熱ゾーン中に搬送され、
−前記粒状材料が前記流通式設備から吐出され、
−前記粒状材料は、少なくとも70%が前記接触型ヒーターから来る、または2つ以上の接触型ヒーターの場合は前記複数の接触型ヒーターから来るエネルギー入力によって加熱され、
−任意選択で、不活性ガスの流れが前記加熱ゾーンの1つまたは複数に加えられ、もしあれば各加熱ゾーン中の前記不活性ガスの流れが、多くとも2の質量比G/M(Gは単位kg/時の前記不活性ガス流量であり、Mは単位kg/時の前記粒状材料の流量である)であるという条件を満たす、方法。 - 前記熱処理法が、乾燥ステップ、予備結晶化ステップ、アニーリングステップ、または後縮合ステップ、またはこれらの任意の組合せを含む、請求項1に記載の方法。
- 1または複数の加熱ゾーン中の前記質量比G/Mが、多くとも1.5、より好ましくは多くとも1.0、0.8、または多くとも0.6ですらある、請求項1または2に記載の方法。
- 前記粒状熱可塑性材料が、熱可塑性半結晶ポリエステルおよび/または熱可塑性半結晶ポリアミドを含む、請求項1〜3のいずれか一項に記載の方法。
- 前記粒状材料が、繊維強化剤および/または無機充填剤を含む、請求項1〜4のいずれか一項に記載の方法。
- 前記粒状材料を予備結晶化する第一加熱ステップと、前記粒状材料を固体の状態で後縮合する第二加熱ステップとを含めて、少なくとも2つの加熱ステップを含む、請求項1〜5のいずれか一項に記載の方法。
- 粒状熱可塑性材料の固相後縮合(SSPC)のための装置であって、送り部分、吐出し部分、および前記送り部分と前記吐出し部分の間に位置決めされた少なくとも2つの加熱ゾーンを備え、かつ各加熱ゾーンが、互いに規則正しく一定の間隔で配置され、前記加熱ゾーン全体にわたって均一に分布した複数個の面状熱交換エレメントを含む接触型ヒーターを備えた、流通式設備である装置。
- 各加熱ゾーンが、本質的に長方形断面を構成する4つの壁によって密閉されている、請求項7に記載の装置。
- 前記加熱プレートが、1〜12cmの範囲のプレート間隔を有する、請求項7または8に記載の装置。
- 弁および/または他の補助装備を包含する狭まる部分および拡がる部分によって断続的に分断された、本質的に長方形または円形断面を有する少なくとも2つの加熱ゾーンを備えた、請求項7〜9のいずれか一項に記載の装置。
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PCT/EP2009/058607 WO2010003956A1 (en) | 2008-07-11 | 2009-07-07 | Process for heat treatment of semi-crystalline polymers |
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JP2022510810A (ja) * | 2018-12-21 | 2022-01-28 | ディーエスエム アイピー アセッツ ビー.ブイ. | 連続固相重合方法及びそこで使用するための反応器カラム |
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DE102009032390A1 (de) * | 2009-07-08 | 2011-01-13 | Coperion Gmbh | Vorrichtung zum Kühlen von Schüttgut sowie Verfahren zum Behandeln von Schüttgut |
DE102012213796B4 (de) * | 2012-08-03 | 2021-03-25 | Brandt Kantentechnik Gmbh | Verfahren und Vorrichtung zum Beschichten von Werkstücken |
CN103264457A (zh) * | 2013-05-31 | 2013-08-28 | 常熟市金泉化纤织造有限责任公司 | 一种防止聚苯硫醚切片干燥过程中氧化的连续干燥方法 |
CN104437265B (zh) * | 2014-11-19 | 2017-03-01 | 济南大学 | 环己酮自缩合反应的制备装置 |
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WO2019141672A1 (en) * | 2018-01-17 | 2019-07-25 | Borealis Ag | Process for obtaining low volatile plastomers |
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WO2010003956A1 (en) | 2010-01-14 |
EP2300142B1 (en) | 2014-03-26 |
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CN102089072B (zh) | 2013-10-23 |
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US9242218B2 (en) | 2016-01-26 |
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