TW202225294A - 藉由在高水溫下水下造粒來生產基於高溫聚合物的顆粒以用於生產（剛性）粒子發泡體 - Google Patents

藉由在高水溫下水下造粒來生產基於高溫聚合物的顆粒以用於生產（剛性）粒子發泡體 Download PDF

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TW202225294A
TW202225294A TW110129942A TW110129942A TW202225294A TW 202225294 A TW202225294 A TW 202225294A TW 110129942 A TW110129942 A TW 110129942A TW 110129942 A TW110129942 A TW 110129942A TW 202225294 A TW202225294 A TW 202225294A
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克利斯汀 特瑞瑟
梅蘭妮 尼珀特
弗洛里安 霍夫
丹尼斯 霍林
莫娜 甘勞夫
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德商贏創運營有限公司
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Abstract

本發明係關於一種使用水下造粒系統從聚合物組成物中之至少一種具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物生產(剛性)粒子發泡體的方法。

Description

藉由在高水溫下水下造粒來生產基於高溫聚合物的顆粒以用於生產（剛性）粒子發泡體
本發明係關於一種使用水下造粒系統從聚合物組成物中之至少一種具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物生產(剛性)粒子發泡體的方法。
由於其高的處理溫度，工業塑膠能根據先前技術，僅藉由繩股(strand)造粒被處理。所得之圓柱形顆粒具有銳利邊緣。在輸送及進一步處理期間，這些銳利邊緣使塵粒和細粒子的形成增加，而需要合適之職業安全措施。該經造粒材料之品質也降低，因為能對該顆粒表面造成破壞，例如微觀的裂痕。 這些問題在某一程度上被WO2005/056653所述之水下造粒所解決。然而得自該方法之顆粒的表面瑕疵(凹痕)的比例增加且有時甚至該顆粒內部之瑕疵(空泡)的比例增加。 為移除低階的經造粒材料，需要費力的下游淘選方法。EP3377288和EP2361174描述藉由在處理池中的水下造粒來生產粒化塑膠材料的方法，在該池中，該處理流體具有高於120℃之溫度，在至少2.0巴之處理壓力下。然而，該經造粒塑膠材料之品質對很多用途是不足的。 原則上有多種手段來生產粒子發泡體。 WO2019/038213描述一種方法，其中利用具有穿孔板之擠出機，將由80wt%至99.5wt%之PEI、0.5wt%至10wt%之發泡劑和0wt%至10wt%之添加劑所組成之組成物處理成經發泡或可發泡之經造粒材料。在取入區與螺桿尖端之間的溫度較佳在320與400℃之間的範圍內。此外，在此段距離之間經常沒有均勻溫度，而是例如在該聚合物熔體之進料方向上有上升溫度之梯度。該穿孔板之溫度是在250與350℃之間且經過該穿孔板而在出口的熔體溫度是在230與360℃之間。通常在該擠出機中裝填該發泡劑。只要在該水下造粒中之壓力低於該發泡劑之膨脹力，該經造粒材料在離開該穿孔板時進行發泡。該膨脹之經造粒材料然後較佳地後續進一步處理成粒子發泡體模製物。因為這些發泡體珠粒經常具有極低密度，所引用之方法尤其負面地影響經濟的輸送。再者，膨脹之粒子發泡體必須在處理成模製物期間總是被壓縮以避免瑕疵和孔洞而不可避免地使密度增加及因此使輕質構造的可能性降低。 WO2019/025245描述一種包含發泡劑且是基於高溫熱塑膠的可膨脹顆粒的生產方法。在此方法中，聚合物熔體係藉由以下方式生產：熔化具有至少180℃之玻璃轉換溫度的聚合物，且在擠出機中300℃與350℃之間的溫度下，與至少一種成核劑混合。在將該發泡劑添加至該聚合物熔體之後，將該熔體冷卻至180℃與250℃之間的溫度，傳輸經過穿孔板且在具有75℃與99℃之間的水溫的水下造粒機中造粒。 必要的噴嘴溫度相較於該一般水溫(低於100℃)是極高的。這對該噴嘴造成冷卻效果且因此導致該聚合物熔體在該噴嘴中凍結的風險，尤其是在該方法啟動時。 在Kunststoffe, 2, 2016出版之Gloeckner und Müller的論文『Brillianten aus dem Reaktor』[得自反應器之鑽石]描述一種意欲防止聚合物熔體在該擠出機噴嘴中凍結的新穎方法。該論文題及多種塑膠。然而不討論粒子發泡體的生產，尤其是從含發泡劑之聚合物熔體生產。
問題 本發明所解決之該先前技術的問題是提供一種高溫粒子發泡體之新穎造粒方法。 解決方法 該問題係藉由提供一種使用水下造粒系統從包含至少一種具有至少180℃之根據ISO 11357-2(出版：2014-07)的玻璃轉換溫度的聚合物之聚合物組成物生產(剛性)粒子發泡體的方法所解決，該方法的特徵在於將擠出機中之聚合物熔體 a)輸送至經加壓之第一水迴路中，壓力係在5至30巴之範圍內且在該水迴路中之水溫是在100℃至200℃範圍內， b)造粒，且 c)隨意地供應至第二水迴路中，該第二水迴路具有低於100℃之溫度且係 1)在未加壓下操作或 2)在5至30巴之範圍內的壓力下操作。 在本發明之具體例中，該聚合物組成物能在離開該擠出機時被導至水下造粒機中。 設計該水下造粒機以在溫度和壓力之組合下操作，使得有密閉系統存在。根據本發明，在該第一水迴路中的溫度是100℃至200℃。經由此措施，在該聚合物熔體與水下造粒機中之處理水的溫度之間的大溫差被最小化。因此能避免在該先前技術中所描述之噴嘴中凍結該聚合物熔體的風險因此能被避免。 在傳統方法中，將來自該擠出機之聚合物熔體供應至在低於100℃之水溫下操作之水下造粒系統。這使該經造粒材料突然冷卻。該顆粒因此在該經造粒材料之表面上發生凹痕或發生空泡。 令人驚訝地發現：根據本發明之程序的結果是在該第一水迴路中提高的溫度水平可能防止形成凹痕或空泡。 根據本發明，經加壓之該第一水迴路較佳在5至30巴，更佳在3至10巴之範圍內的壓力下操作。在該第一水迴路中之水溫較佳是100℃至200℃，更佳是105至180℃。 密閉之經加壓的水循環系統使操作能在較高水溫下進行，同時使操作人員減少暴露於熱蒸氣。 在該第一水迴路中進行造粒。這抑制因該先前技術中所述之劃傷及尖銳破裂邊緣所致之塵粒形成以及該經造粒材料品質降低的缺點。 根據本發明，能將所得之經造粒材料供應至具有低於100℃之溫度且未加壓地被操作或在5至30巴之壓力下操作的第二水迴路。 當根據方法步驟c)2)之該第二水迴路係在壓力下操作時，該壓力水平在將該經造粒材料從該處理水中分離出之前被降至周圍壓力。 可將所得之該經造粒材料供應至乾燥方法。 可以使用一般乾燥器進行乾燥。適合此目的者是例如離心乾燥器、循環空氣乾燥器、加壓空氣乾燥器、衝擊乾燥器、帶式乾燥器、吸附乾燥器、具有紅外加熱之旋轉鼓或含分子篩之乾燥器。 在替代之方法變化型中，所得之經造粒材料在方法步驟a)及b)之後立即從該經加壓的第一迴路排出且供應至乾燥方法。當所得之經造粒材料意欲在較高溫度水平下進行進一步處理時是特別有益的。 在該具體例之進一步變化型中，可以利用擠出機加工含發泡劑之聚合物組成物。 在該變化型中，該聚合物組成物在離開該擠出機時被導至該水下造粒機中。 設計該水下造粒機以在溫度和壓力的組合下操作，使得發泡之發生得以防止，例如藉由在步驟a)中之溫度比該含發泡劑之聚合物熔體的Tg低至少5℃。這措施提供一種含發泡劑之經造粒材料，其後續可藉由更新輸入能量被發泡成所需密度且/或藉由隨意之模製進一步被加工成粒子發泡體工件。 在該第一水迴路中的壓力(也稱為反壓)防止該發泡劑沸騰，從而防止顆粒發泡。 適合此目的之發泡劑係選自下列群組：在常壓下之沸點低於該基礎材料之玻璃轉換溫度的揮發性有機化合物、無機發泡劑、熱可分解之發泡劑及彼等之混合物。在常壓下之沸點低於該基礎材料之玻璃轉換溫度且在常溫(亦即25℃，1013毫巴)下為液態的揮發性有機化合物較佳係選自下列群組：非鹵化之烴、酮、醇、鹵化烴及彼等之混合物。 酮較佳係選自丙酮、甲基乙酮、環己酮、環壬酮、二丙酮醇及彼等之混合物。酮更佳係選自丙酮、甲基乙基酮及彼等之混合物。 具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的適合聚合物係選自聚碸或聚醯亞胺之群組，尤其是聚醚碸(PESU)、聚苯碸(PPSU)、聚碸(PSU)、聚醚醯亞胺(PEI)、熱塑性聚醯亞胺及其混合物。以PEI和PEEK之摻合物為底質之粒子發泡體也是適合的。 除非另外陳明，所述之玻璃轉換溫度是根據本發明，藉由DSC(微分掃描卡計)所測量的。精於此技術者知道：僅在第一加熱循環達到一個比最高玻璃轉換或熔化溫度高最少25℃但比材料之最低分解溫度低至少20℃的溫度之後，當該材料樣品保持在此溫度至少2分鐘時，DSC資訊才充足。該樣本然後冷卻回到比待測定之最低玻璃轉換或熔化溫度低至少20℃的溫度，其中冷卻速率應不高於20℃/分鐘，較佳不高於10℃/分鐘。在進一步等待數分鐘之後，進行實際測量，其中以通常10℃/分鐘或更低之加熱速率，將該樣本加熱至比該最高熔化或玻璃轉換溫度高至少20℃。 在用於生產粒子發泡體之方法的另外變化型中，將處理含成核劑之對應的聚合物組成物。 該隨意之成核劑較佳係選自由滑石、石墨、碳黑、二氧化鈦及彼等之混合物組成之群組。該隨意之成核劑有利地改良泡囊(cell)形態。 該聚合物組成物含有以總質量計0.01重量%至3重量%，較佳地0.05重量%至1重量%之成核劑。 根據本發明所生產之顆粒被進一步加工成(剛性)粒子發泡體。 (剛性)粒子發泡體在本文是指發泡體、剛性發泡體、粒子發泡體和剛性粒子發泡體，其係基於具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物所生產。 由於該等顆粒之較好品質，尤其，在經造粒材料中或在該顆粒表面上的瑕疵的最小化，獲得具有特別均勻之孔隙尺寸分布的(剛性)粒子發泡體。 根據本發明之方法，從至少一種具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物所生產之該(剛性)粒子發泡體係用於太空載具或航空載具之建構、造船、鐵道載具建構或載具建構(尤其是電動裝置)中、或於其外裝中。這些(剛性)粒子發泡體也能用於生產同樣能用在該等應用的複合材料。 從至少一種具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物所生產的(剛性)粒子發泡體也另外特別適合併入航空載具外裝中。該『外裝』不僅是指在航空載具之外殼中，而是也特別在航空載具機頭中，在尾部區中、在該外側門中、在該控制面中或在轉子葉片中作為填料。 尤其，其低的可燃性意味著根據本發明所製造之(剛性)粒子發泡體及複合材料也能被安裝在該載具內部中。 以具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物為底質之(剛性)粒子發泡體特別適合併入航空載具的內裝中。除了噴射機或輕航機之外，航空載具也包括直升機或甚至是航太載具。在此種航空載具之內裝中的裝設實例是例如在客機之座椅後側能被折疊的托盤、用於座椅或內部隔板的填料，以及例如也用於內門中。 本方法及利用彼所產生之(剛性)粒子發泡體特別適合高溫用途。
實例1 Ultem 1000型聚醚醯亞胺之水下造粒 聚醚醯亞胺(PEI)(Ultem 1000，荷蘭SABIC)被裝填在擠出機(自動單螺桿APM E1-180)之儲存槽中。在約370至375℃及15巴之壓力下進行該擠出。通過量是160kg/h。該熔體經由穿孔板被供應至水下造粒系統(Sphero 70，德國MAAG Automatik GmbH)。在該穿孔板上游之噴嘴中的壓力約195巴。利用9刀，以2000升/分鐘進行該造粒。 在二個處理水迴路中進行該水下造粒。在第一的高溫迴路中，該處理水溫在約4.95巴之壓力下約140℃。在第二迴路中，該處理水溫在約2.5巴之壓力下約70℃。在該二迴路中之滯留時間各是約8秒。 該經造粒材料然後在離心乾燥器(Centro 300，德國MAAG Automatik GmbH)乾燥。殘餘水含量是0.30%至0.47%。

Claims (10)

  1. 一種使用水下造粒系統從包含至少一種具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物之聚合物組成物生產(剛性)粒子發泡體的方法，其特徵在於將擠出機中之聚合物熔體 a)輸送至經加壓之第一水迴路中，壓力係在5至30巴之範圍內且在該水迴路中之水溫是在100℃至200℃範圍內， b)造粒，且 c)隨意地供應至第二水迴路中，該第二水迴路具有低於100℃之溫度且係 1)在未加壓下操作或 2)在5至30巴之範圍內的壓力下操作。
  2. 如請求項1之生產(剛性)粒子發泡體的方法，其中該具有至少180℃之根據ISO 11357-2的玻璃轉換溫度的聚合物係選自聚碸或聚醯亞胺之群組，尤其是聚醚碸(PESU)、聚苯碸(PPSU)、聚碸(PSU)、聚醚醯亞胺(PEI)、熱塑性聚醯亞胺及其混合物。
  3. 如請求項1之生產(剛性)粒子發泡體的方法，其中該聚合物組成物包含發泡劑。
  4. 如請求項3之生產(剛性)粒子發泡體的方法，其中在步驟a)中之溫度比含該發泡劑之聚合物熔體之Tg低至少5℃。
  5. 如請求項3之生產(剛性)粒子發泡體的方法，其中該發泡劑係選自由揮發性有機化合物(其沸點在常壓下低於該基礎材料之玻璃轉換溫度)、無機發泡劑、可熱分解之發泡劑及以上物質之混合物所組成之群組。
  6. 如請求項1之生產(剛性)粒子發泡體的方法，其中該聚合物組成物包含成核劑。
  7. 如請求項6之生產(剛性)粒子發泡體的方法，其中該成核劑係選自由滑石、石墨、碳黑、二氧化鈦及以上物質之混合物所組成之群組。
  8. 如請求項1之生產(剛性)粒子發泡體的方法，其中所得之經造粒材料係在步驟b)後被排出且供應至乾燥方法。
  9. 如請求項1之生產(剛性)粒子發泡體的方法，其中所得之經造粒材料係在步驟c)後被排出且供應至乾燥方法。
  10. 一種藉由請求項1之方法所生產之(剛性)發泡體的用途，其係在航太工業中用於船舶建造、用於載具建構，尤其是在電動裝置中。
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EP4200111A1 (de) 2023-06-28
WO2022037857A1 (de) 2022-02-24
IL300381A (en) 2023-04-01
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