CN1842406A - 由缩聚物制备成型体的方法 - Google Patents

由缩聚物制备成型体的方法 Download PDF

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Publication number
CN1842406A
CN1842406A CNA2004800247780A CN200480024778A CN1842406A CN 1842406 A CN1842406 A CN 1842406A CN A2004800247780 A CNA2004800247780 A CN A2004800247780A CN 200480024778 A CN200480024778 A CN 200480024778A CN 1842406 A CN1842406 A CN 1842406A
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China
Prior art keywords
condensation polymer
extruder
fusion
melt
less
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CNA2004800247780A
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English (en)
Inventor
A·克里斯特尔
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Gebr RUEHLER AG
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Gebr RUEHLER AG
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Publication of CN1842406A publication Critical patent/CN1842406A/zh
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/88—Post-polymerisation treatment
    • C08G63/90—Purification; Drying
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Abstract

本发明涉及一种由缩聚物，特别是聚酯，例如聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸丁二醇酯(PBT)或它们的共聚物制备成型体，特别是型材的方法，在此缩聚物在方法过程中熔融和随后又固化，其特征在于，缩聚物的温度在方法过程中高于缩聚物的熔融温度的总时间为少于约60秒。该方法优选借助多螺杆挤出机进行，其中缩聚物在固体状态下的脱气和/或干燥在低于大气压的压力下和/或加入惰性气体条件下进行。缩聚物在挤出机中熔融后仍在挤出机中停留的时间段少于约15秒。

Description

由缩聚物制备成型体的方法
本发明涉及由缩聚物，特别是聚酯，如聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸丁二醇酯(PBT)或它们的共聚物制备成型体，特别是型材的方法，在此缩聚物在方法过程中熔融和随后又固化。
特别是应用PET的这种方法是已知的。在此PET起始材料直接来自PET-合成，或应用回收物，特别是PET-瓶子回收物(RPET)，在此用洗涤和粉碎后得到的碎片或薄片进行操作。这些碎片除了含有可能的其他的不期望的杂质外总是含有少量的水，在此其一方面可能是在瓶子洗涤过程中没弄干净的残留水和/或可能是在碎片储存和运输时新进入的水。假如这些具有水含量的来自RPET或新的PET的碎片在挤出机中熔融以制备成型体，那么缩合反应主要向着相反的方向(平衡调节)进行，和水解作用占主导，以致于平均链长，也就是聚合度减小，这样聚合物的粘度(作为粘度指数或特性粘度(IV)给出)就减小了。这种水解降解越显著，为降解反应提供的水和时间越多。
在现有技术中迄今为止的努力是减少水含量。在此常用的预干燥方法立求下降至100ppm以下(典型为约30ppm)的水含量的较小值，以阻止在随后的PET和/或RPET熔融时在熔融状态下通常的停留时间内发生太强烈的IV减少，在熔融状态下缩聚物的反应速度是值得提到的。从约0.80到约0.75大约0.05的IV减少量是可接受的。当追求包括整合的预干燥的连续操作时，这种大规模的预干燥需要较多的时间和能量并使得开头所述的方法变得缓慢。
也符合现有技术的是，将熔融的PET和/或RPET较长时间地置于几个mbar或甚至小于1mbar的熔体真空中，以使得熔体脱去在缩聚反应中释放的水分，从而提高聚合度。然而一个这样的过程对于具有高粘度的聚酯和特别也对于洗涤的瓶子碎片形成的RPET是不合适的，因为缩聚反应同时也总是伴随着降解反应，这导致产物性能变差，如发黄或含有乙醛。
在DE10054226中描述了一种方法，在该方法中通过合适地选择过程参数，特别是停留时间和任选的受限制的预干燥，使得水解降解减小至最小。然而这一方法只描述了颗粒或随后切成颗粒的线材的制备。其也描述了一种中间产物的制备，该中间产物必须再一次地熔融，以由此制备产物，在此产物的形状与颗粒的形状无关。这样就有这样的缺点，即缩聚物总共至少必须要熔融两次和由此缩聚物保持在熔体中的总的时间延长，这在制备最终产品时导致了总体上较高的降解。
所以本发明的任务是，这样发展现有技术的方法，使得在只有部分预干燥时也不出现比现有技术更大的IV减少量，使导致产品性能变差的进一步的降解反应减小至最小，通过该方法可直接制备成型体，由这些成型体可以无需再次熔融地制备最终产品。
由此产生的优点是，可由缩聚物起始材料以缩聚物在熔体中最少的总停留时间而制备产品和从而水解的和热氧化的降解总体上减小至最小值。这导致了例如改善的色彩和在聚对苯二甲酸乙二醇酯(PET)加工时产生较小的乙醛含量。
作为成型体或型材指的是最终产品或半产品，它们通过加工步骤，如切割、弯曲或深冲等而可转变成最终产品。最终产品的形状在此相应于成型体的形状或是直接由成型体的形状导出。
例如可由复杂的型材棒通过多个部件的切割和互相接合制备框架。也可以由圆的型材棒，通过型材棒基本上是横向着制备方向切割，制成圆的片或板。另一个例子是由薄膜或板材制备空心体，如杯或桶，是通过薄膜或板材在成型工具中或其上压制或拉制。在此必需的是，缩聚物成型体加热至软化温度。然而加热不能超过缩聚物的熔点。空心体又可以为最终产品或半成品，其例如通过拉伸吹制成形再次进行形状匹配。
这一任务通过根据权利要求1的方法解决。在此将所要加工的缩聚物处于熔体中和在熔融温度或以上的时间控制在少于60秒。这样缩聚物不再有足够的时间，而由于它的较高的水分进行主要水解的反应。从而可以至少部分地不用进行费时的和耗能的预干燥，和尽管在起始缩聚物中有较高的水含量，在熔融状态下加工时还是明显少地出现水解。所以例如对于PET或RPET来说IV-降解即使在较高的约600ppm的水含量时还可保持在小的可接受的值。
优选地，在根据本发明的方法中缩聚物的温度在方法过程中处于缩聚物的熔融温度以上的总时间保持在约30秒以下。在此可以允许在熔体中以多于200ppm(w/w)的残留水含量进行操作，而不必用多于0.05的IV-减少量作为代价。
对于许多应用优选使用聚对苯二甲酸乙二醇酯(PET)作为缩聚物。
缩聚物的起始形式作为具有200-950kg/m3的堆密度的松散材料，特别以颗粒、粉末或碎片或薄片的形式存在，在此后者典型地为瓶子回收物(RPET)。
优选地，缩聚物起始材料在熔融前部分地进行预干燥。这样通过不太昂贵的部分干燥和在熔融状态下的短的停留时间的组合而可得到具有较小的IV降解的最终产品。
在特殊的实施方案中本方法具有用来从缩聚物中去除挥发性的杂质和/或分解产物的除气步骤。
对于缩聚物的熔体，优选应用双螺杆或多螺杆挤出机，特别是环形挤出机。对于环形挤出机，对所要加工的产品产生有利影响的表面和所要加工的产品的体积之间的比例是特别地大，以致于在预先给定的工作面长度下达到较高的脱气效率和窄的停留时间谱，和最后达到比用传统的双螺旋挤出机总体上更短的停留时间。
优选地，缩聚物以固态输送入挤出机中，和缩聚物被加热到熔点以下的温度，在此缩聚物脱气和/或干燥。在此固态的缩聚物的脱气和/或干燥在大气压以下的几个mbar(典型地为20-300mbar)的压力下和/或在加入惰性气体条件下进行。
特别地，根据本发明的方法突出之处在于，缩聚物在方法过程中作为熔体存在的总时间是由缩聚物在挤出机中熔融后仍在挤出机中停留的第一时间段和仍是熔融的缩聚物在挤出机外被加工的第二时间段一起计算的，在此第一时间段优选为少于约15秒。特别有利的是熔体在挤出机中的停留时间为少于约10秒。
假如加工RPET或只有较少预干燥的PET，那么这可能具有优点的是，在挤出机中熔融后进行熔体脱气，以从熔体中去除可能的杂质和一部分溶解的水分。在此几十mbar的绝对压力(典型地为30-130mbar)的真空度是足够的。压力的进一步降低常常是不必要的和从而出于工艺成本的原因也是不期望的。尽管如此，为了在短时间内降低所要分离的杂质的分压，可以使用只有几个mbar或甚至在1mbar以下的绝对压力的真空度。
根据本发明的方法也适合于用来加入添加剂。
添加剂可以在熔融之前加入，或者与缩聚物一起加入或者通过独立的计量-和加料装置加入。在此添加剂在熔融时通过捏合元件13同时最佳地混合。添加剂也可以在挤出机中熔融后加入。添加剂的加入例如通过侧面加料装置进行。另外还可在挤出机中选择性地具有捏合-或混合元件，以便最佳地混合添加剂。在特别的情况下添加剂也可以在挤出机后才加入。
作为添加剂合适的例如是染料和颜料、UV阻断剂、加工辅助剂、稳定剂、冲击改性剂、化学和物理型的发泡剂、填料如成核剂、阻挡层或改善机械性能的颗粒、增强体，如球体或纤维，以及反应物质，如氧吸收剂、乙醛吸收剂或提高分子量的物质等等。
添加剂可以单独地加入或作为添加剂包的组成部分加入。为了制备添加剂包，要使用多种添加剂。另外可以应用所有的添加剂都可以加入其中的载体材料。添加剂包不仅可以作为均匀的粉末或颗粒也可以作为简单的添加剂混合物存在。
经熔融的缩聚物在挤出机外(第二时间段)的加工可以含有用来分离杂质颗粒的熔体过滤步骤。为了构成必需的压力，优选使用熔体泵。在此熔体泵和熔体过滤器这样整合到工艺中，使得根据本发明的短的停留时间得到保证。
用来成型的步骤和用来随后冷却到缩聚反应的逆反应基本上停止的温度的步骤也都属于第二时间段。
在此成型的步骤典型地在挤压通过缩聚物熔体的喷嘴中进行。可以使用各种不同形状的喷嘴出口孔。可以使用简单的形状，如圆形的、环形的或多角的，特别是基本上是矩形的或也可以是复杂的形状。对于基本上矩形的喷嘴出口孔，通过其高的宽度和高度的比例(如B∶H≥10)而形成带状的成型体。对于较小的宽度与高度的比例(如B∶H＜10)生成基本上是矩形的型材。对于非带状的、复杂的喷嘴出口孔通常也给出较小的宽度与高度的比例，这样就生成型材。这样的复杂的型材具有至少一个接合面，其与另一个接合面构成一个角度。
以宽度和高度测得的成型体的大小是由喷嘴出口孔的尺寸和可能的后成形过程步骤，如拉伸或收缩给出的。为了拉长到成型体所期望的形状，通常已知的是，喷嘴出口孔的形状这样与所要加工的缩聚物的性能相匹配，以致于喷嘴出口后可能的形状改变例如通过线材扩张而补偿。
通常地，至少喷嘴出口孔和特别是成型体的宽度或高度为大于10mm，特别是大于25mm。对于具有大的宽度与高度比例的成型体，其宽度是大于100mm，特别是大于250mm。另一方面具有优点的是，成型体的至少一个延长不超过100mm，特别是50mm，因为否则在成型体的外壁和中心之间的冷却就要太不一样了。
成型体的长度根据成型体基本上横对着制备方向切割的次数频率给出。长度在此可以比宽度或高度大几个数量级，例如对于薄膜或带材来说情况如此。对于型材棒，其长度总是显著超过其长度或宽度。对于圆盘或块材，成型体的长度可以小于其宽度或高度，或至少在与其宽度或高度相当的数量级。
当所有的缩聚物已经下降到缩聚物的熔融温度Tm以下时第二时间段结束。在此应进行快速冷却。
从缩聚物离开喷嘴时的熔体温度(TD)初始冷却到冷却温度(Ta)以大于300℃/Min，优选大于600℃/Min，特别优选为大于1200℃/Min的冷却速率进行，在此Ta＝0.9*Tm。冷却可以通过冷却介质，如水或液氮，或通过与冷的表面接触，如冷却辊或在型材周围的冷却夹套接触而进行。假如应用冷却装置，其结构上与喷嘴相连接，那么适合作为喷嘴区域向冷却区域的过渡的是装置的温度下降到缩聚物的熔融温度以下的地方。
首先对于较厚的成型体，起始较高的冷却速率具有重要意义，不仅是为了保持在喷嘴外的附加的停留时间较少，而且因为降解在成型体的内部和外部严重不同地进行。然后在进一步的工艺过程中，为了阻止应力，成型体可小心地被冷却或甚至有目的地调节温度，在此应避免较长时间地超过冷却温度Ta。随后成型体例如可卷绕、变形、冲压或切成一定长度和/或宽度的部件。
本发明的一个特征是，通过根据本发明的方法可由聚对苯二甲酸乙二醇酯以较小水解降解和具有非常少量的乙醛制备成型体。所以可能的是，制备具有少于3ppm，特别是少于2ppm乙醛的成型体，而成型体不必为了去除乙醛而进行一个调节步骤。
本发明的其他的优点、特征和应用可能性现在根据附图由下面的所解释的不受限制的实施例的描述来给出，在此：
图1示出了对于PET在熔融状态下从0.81到0.76的IV-降解所允许的停留时间作为PET-熔体的残留水含量的函数；
图2a-2e示出了对于可能的简单的成型体或型材几何形状的例子；和
图3a-3d示出对于可能的复杂的成型体或型材的几何形状的例子。
图1示出了对于PET在熔融状态下从0.81到0.76的IV-降解所允许的停留时间作为PET熔体的残留水含量的函数。在此给出了在285℃熔融温度下在部分预干燥下的允许的停留时间，其限制IV-降解到对于许多应用可接受的值0.05。如开头所述，与此不同的是，在现有技术中要预干燥至100ppm以下。
图2a-2e示出了对于可能的简单的成型体或型材几何形状的例于。
图2a示出了具有矩形形状横截面的成型体或型材，在此比例B∶H是大的，如＞10。这是带状型材。
图2b示出了具有圆形横截面的成型体或型材。这是圆形型材。
图2c示出了具有圆环形状横截面的成型体或型材。这是带状型材。
图2d示出了具有矩形形状横截面的成型体或型材，在此比例B∶H是小的，如约1∶1-3∶1。这是棒状型材。
图2e示出了具有矩形形状横截面和具有成斜面的棱边的成型体或型材。这是条形(Leisten)型材。
图3a-3d示出了对于可能的复杂的成型体或型材几何形状的例子，在此图3a是十字形型材，图3b是燕尾槽形型材，图3c是角形型材和图3d是U形型材。
除了成型体或型材外采用根据本发明的方法也可以制备薄膜或带材。在此薄膜优选具有约200μm的厚度和尤其用作为柔韧的包装薄膜。根据本发明所制备的带材优选具有大于200μm的厚度，然而也可以是超过800μm厚。这种带材的最大厚度为约5mm。其特别地用作为刚性或半刚性包装材料。
实施例1
用锑催化剂制备的聚对苯二甲酸乙二醇酯颗粒，其具有起始特性粘数为0.84dl/g和600ppm的水分含量，在30mm环形挤出机中熔融和脱气，并随后采用齿轮泵通过型材喷嘴而输出。型材直接在喷嘴出口后面冷却。由型材制备具有约40mm直径和约5mm厚的圆盘。生产能力为200kg/h。在挤出机中熔融状态下的停留时间为约4秒和在挤出机后面熔融状态下的停留时间为约12秒。
所制备的圆盘具有0.79-0.80dl/g的特性粘数和1.5-1.8ppm的乙醛含量。
实施例2
用锗催化剂制备的聚对苯二甲酸乙二醇酯颗粒，其具有起始特性粘数为0.75dl/g和2000ppm的水分含量，在30mm环形挤出机中熔融和脱气，并随后采用齿轮泵通过型材喷嘴而输出。型材直接在喷嘴出口后面冷却。由型材制备具有约40mm直径和约5mm厚的圆盘。生产能力为200kg/h。在挤出机中熔融状态下的停留时间为约4秒和在挤出机后面熔融状态下的停留时间为约12秒。
所制备的圆盘具有0.71-0.72dl/g的特性粘数和2.0-2.5ppm的乙醛含量。
实施例3
聚对苯二甲酸乙二醇酯颗粒如在实施例2中那样加工。生产能力为120kg/h。在挤出机中熔融状态下的停留时间为约6秒和在挤出机后面熔融状态下的停留时间为约18秒。
所制备的圆盘具有0.72dl/g范围的特性粘数。
实施例4
聚对苯二甲酸乙二醇酯颗粒如在实施例2中那样加工。生产能力为250kg/h。在挤出机中熔融状态下的停留时间为约3秒和在挤出机后面熔融状态下的停留时间为约10秒。
所制备的圆盘具有0.71dl/g范围的特性粘数。

Claims (23)

1、一种用来由缩聚物制备成型体，特别是型材的方法，在此缩聚物在方法过程中熔融和随后又固化，其特征在于，缩聚物的温度在方法过程中高于缩聚物的熔融温度的总时间为少于约60秒。
2、根据权利要求1的方法，其特征在于，缩聚物的温度在方法过程中高于缩聚物的熔融温度的总时间为少于约30秒。
3、根据权利要求1或2的方法，其特征在于，在熔体中的残留水含量大于200ppm。
4、根据权利要求1-3之一的方法，其特征在于，缩聚物是聚酯，特别是聚对苯二甲酸乙二醇酯，或其共聚物。
5、根据上述权利要求之一的方法，其特征在于，缩聚物的起始形式是作为松散材料，例如以颗粒、碎片或切削料的形式存在和堆密度为200-950kg/m3。
6、根据权利要求4-5之一的方法，其特征在于，聚对苯二甲酸乙二醇酯为瓶子回收物。
7、根据上述权利要求之一的方法，其特征在于，缩聚物起始材料在熔融前部分地预干燥。
8、根据上述权利要求之一的方法，其特征在于，其具有用来从缩聚物熔体去除挥发性的杂质和/或分解产物的脱气步骤。
9、根据上述权利要求之一的方法，其特征在于，使用挤出机用于缩聚物的熔融。
10、根据权利要求9的方法，其特征在于，使用双螺杆或多螺杆挤出机，特别是环形挤出机，用于缩聚物的熔融。
11、根据权利要求9-10之一的方法，其中将缩聚物以固态输入到挤出机中，将缩聚物加热到熔点以下的温度和将缩聚物脱气和/或干燥，其特征在于，固态的缩聚物的脱气和/或干燥是在大气压以下的压力下和/或加入惰性气体下进行的。
12、根据权利要求9-11之一的方法，其特征在于，缩聚物在方法过程中作为熔体存在的总时间包括缩聚物在挤出机中熔融后还在挤出机中停留的第一时间段，和仍是熔融的缩聚物在挤出机外被加工的第二时间段。
13、根据权利要求12的方法，其特征在于，第一时间段的持续时间少于约15秒。
14、根据权利要求13的方法，其特征在于，第一时间段的持续时间少于约10秒。
15、根据权利要求9-14之一的方法，其特征在于，熔融的缩聚物在挤出机外部的加工包括一个熔体过滤步骤。
16、根据权利要求9-15之一的方法，其特征在于，熔融的缩聚物在挤出机外部的加工包括使用熔体泵。
17、根据权利要求9-16之一的方法，其特征在于，熔融的缩聚物在挤出机外部的加工包括使用成型喷嘴。
18、根据权利要求17的方法，其特征在于，成型喷嘴具有出口孔，其具有在至少一个方向(宽度或高度)大于10mm，特别是大于25mm的尺寸。
19、根据权利要求17或18的方法，其特征在于，缩聚物在离开成型喷嘴后以大于300℃每分钟的起始冷却速率冷却。
20、根据权利要求19的方法，其特征在于，缩聚物在离开成型喷嘴以后以大于600℃每分钟，特别是以大于1200℃每分钟的起始冷却速率冷却。
21、根据上述权利要求之一的方法，其特征在于，向缩聚物中混入添加剂。
22、应用根据上述权利要求之一的方法由缩聚物制备的成型体，特别是型材。
23、根据权利要求22的成型体，其特征在于，成型体的平均乙醛含量为小于3ppm，特别是小于2ppm。
CNA2004800247780A 2003-10-14 2004-10-12 由缩聚物制备成型体的方法 Pending CN1842406A (zh)

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