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TW201920405A - 應用於航空器內部中的ｐｅｉ粒子發泡體 - Google Patents

應用於航空器內部中的ｐｅｉ粒子發泡體 Download PDF

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Publication number
TW201920405A
TW201920405A TW107129090A TW107129090A TW201920405A TW 201920405 A TW201920405 A TW 201920405A TW 107129090 A TW107129090 A TW 107129090A TW 107129090 A TW107129090 A TW 107129090A TW 201920405 A TW201920405 A TW 201920405A
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Taiwan
Prior art keywords
foam
weight
particle
pei
particle foam
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TW107129090A
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English (en)
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TWI851541B (zh
Inventor
克利斯汀 特瑞瑟
丹尼斯 霍林
凱 柏恩哈德
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德商贏創羅恩有限責任公司
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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Molding Of Porous Articles (AREA)

Abstract

基於聚醚醯亞胺(PEI)之聚合物發泡體符合航空產業對於航空器內部所要求的法律規範。尤其是，對燃燒特性、對於介質之安定性以及機械性質之需求在此構成相當大的挑戰。根據先前技術，適用之聚合物發泡體係經製造為半成品。再加工以產生成形物件在時間及材料利用方面不經濟，例如，因其有大量裁切廢料。本發明解決此問題的方式在於原則上適用之材料可經加工以產生粒子發泡體模製品。該等模製品可於未有再加工之下以短循環時間來製造，因此具有經濟效益。此外，此造成新的功能整合方法，例如藉由將嵌件等直接併入發泡體，以及關於設計方面的自由度。

Description

應用於航空器內部中的ＰＥＩ粒子發泡體
基於聚醚醯亞胺(PEI)之聚合物發泡體符合航空產業對於航空器內部所要求的法律規範。尤其是，對燃燒特性、對於介質之安定性以及機械性質之需求在此構成相當大的挑戰。根據先前技術，適用之聚合物發泡體係經製造為半成品。再加工以產生成形物件在時間及材料利用方面不經濟，例如，因其有大量裁切廢料。本發明解決此問題的方式在於原則上適用之材料可經加工以產生粒子發泡體模製品。該等模製品可於未有再加工之下以短循環時間來製造，因此具有經濟效益。此外，此造成新的功能整合方法，例如藉由將嵌件等直接併入發泡體，以及關於設計方面的自由度。
適用於航空產業中之安裝的發泡體材料為常識。然而，大部分基於該目的所描述之發泡體係僅由純PMI(聚甲基丙烯醯亞胺)、PPSU(聚苯碸(polyphenylene sulfones))或PES(聚醚碸)所構成。亦於文獻中發現者為PI (聚丙烯醯亞胺(polyarylimide))，惟從毒物學觀點來看其不適合。全部該等材料迄今僅呈塊狀或板狀材料形式使用。
亦較不詳細地描述其他材料作為用於航空產業中之安裝的板狀材料。聚(氧-1,4-苯基磺醯基-1,4-苯基) (PESU)為此種材料之實例。此係例如由DIAB以產品名Divinycell F銷售。然而，在該等擠出發泡體板的進一步加工中，產生不經濟的大量碎料材料。
一種避免製造立體發泡體模製品中之裁切廢料的經濟方法係使用發泡體粒子(珠粒發泡體)而非板材發泡體。根據先前技術可用的全部粒子發泡體均具有在高溫下使用的情況下的缺點或者尤其在高溫下之整體非最佳機械性質。此外，只有非常少數現有發泡體非極易燃，因而能合格地用於公路載具、軌道載具或航空載具內部中之安裝。例如，基於聚丙烯(EPP)、聚苯乙烯(EPS)、熱塑性聚胺甲酸酯彈性體(E-TPU)或PMI(ROHACELL Triple F)之粒子發泡體具有不足的阻燃性，然而原則上適用之全部固有阻燃性聚合物例如PES、PEI或PPSU根據目前的先前技術只能加工以產生板材發泡體。
難題
藉由本發明所克服之關於先前技術的問題係提供用於製造用於航空器建造的新穎發泡體或複合材料之組成物，該等複合材料可包含例如具有熱塑性或交聯外層之發泡體核心。所得之發泡體將具有針對載具及航空器建造領域中許多應用之於高溫下的可用性、良好機械性質(尤其是關於充足的斷裂伸長率)、及至少充足的阻燃性之良好組合。
更特別的是，該發泡體應針對各種液體，酸性、鹼性或疏水性液體，以及針對乳液具有高安定性。
此外，該發泡體將可從廣泛不同方法所發展的組成物實現以及具有廣範圍的立體形狀，而且在最終組件之製造中，若產生任何碎料材料，僅有極少量碎料材料。
另外的不明確問題可從本文內容中之說明、申請專利範圍或實例暸解，此處不為此目的而明確列舉。

解決方案
該等問題係藉由提出用於製造航空產業(尤其用於航空器建造)中使用的低可燃性熱安定性發泡體材料之新穎組成物而解決。用於製造發泡體之本發明組成物的特徵在於其包含基於聚醚醯亞胺(PEI)之粒子發泡體。根據本發明之作為發泡材料的粒子發泡體具有介於180與215℃之間的玻璃轉化溫度，以及其中之粒子發泡體的平均孔室直徑係小於2 mm，較佳係小於1 mm，更佳係小於500 μm以及最佳係小於250 μm。
此尤其令人意外的原因是，該PEI之實際玻璃轉化溫度為215至217℃，以及該材料因此無法根據當前的先前技術(例如藉由水下造粒(underwater pelletization))加工以產生粒子發泡體。
根據本發明，用語「孔室(cell)」描述發泡體中不含任何基質材料但至少部分被基質材料包圍的區域。孔室於此處亦稱為孔(pore)。理想情況下，於剛性發泡體中，該等孔或孔室為封閉式，其又意味著該孔室完全被發泡體之基質材料包圍。在較軟發泡體的情況下，至少某種程度地存在開放式孔室。不過經由不完整壁之排列或在條狀的極端情況下，此等被認定為個別孔室。因此亦可能測定此等開放式孔室的大小。於許多情況下孔室之大小可以簡單方式測量，例如借助於顯微鏡測量。亦考慮該等因素，熟習本領域之人士可依從發泡體中之最大孔室大小。
根據本發明應暸解發泡體粒子意指藉由個別未發泡或預發泡粒子之發泡所界定的粒子發泡體中之區域。彼此黏接之個別發泡體粒子之間的邊界容易肉眼看出或在光學顯微鏡下測定。當兩個發泡體粒子之間的邊界很明顯時，此尤其適用。然而，由於不一定是該情況，本發明使用簡化方法：基於該目的，以簡單方式從未發泡粒子之直徑、未發泡粒子之總體積及成品發泡體部件的體積計算發泡體粒子之理論平均直徑。熟習本領域之人士明白，在粒子發泡體的情況下，發泡體粒子之規則大小分布可以在發泡體部件之邊緣區域中僅發生少許偏差的方式獲致。本發明之另一優點係介於個別發泡體粒子之間的間隙之體積比例小到於成品發泡體部件之體積測量中幾乎不表現出來。較佳的，成品發泡體中之發泡體粒子小於1 cm，更佳係小於0.7 cm。
根據本發明，除非另外說明，否則所報告之玻璃轉化溫度係利用DSC (微差掃描熱量測定法)測量。在這方面，熟習本領域之人士明白DSC只有當第一次加熱循環高達高於材料的最高玻璃轉化或熔化溫度至少25℃但低於最低分解溫度至少20℃的溫度之後才充分確定，該材料樣本於該溫度下保持至少2分鐘。之後，將該樣本冷卻回低於待測定之最低玻璃轉化或熔化溫度至少20℃，其中冷卻速率不應超過20℃/min、較佳不超過10℃/min。於另外數分鐘的等待時間之後，進行實際測量，其中該樣本係以通常為10℃/min或更低之加熱速率加熱至高於最高熔化或玻璃轉化溫度至少20℃。
較佳的，於本發明之第一替代實施態樣中，用於製造粒子發泡體之本發明組成物係由80重量%至99.5重量%之PEI組成。此外，該組成物包括0.5重量%至10重量%、較佳為1重量%至9重量%之發泡劑。其可進一步包含尤其是0重量%至10重量%、較佳為1重量%至5重量%之添加劑。
該等添加劑尤其可為阻燃劑、塑化劑、顏料、UV安定劑、成核劑、耐衝擊性改質劑、黏著促進劑、流變改質劑、鏈增長劑、纖維及/或奈米粒子。
所使用之阻燃劑通常為磷化合物，特別是磷酸酯、膦或亞磷酸酯。適用之UV安定劑及/或UV吸收劑在本技術中為一般常識。HALS化合物、Tinuvin類或三唑類通常用於該目的。所使用之耐衝擊性改質劑通常為包含彈性及/或柔軟/撓性相之聚合物珠。該等聚合物珠經常包含具有本身不超過輕度交聯之外殼的核-(殼-)殼珠，以及純聚合物會展現與PEI之至少最小溶混性。原則上可使用任何已知顏料。大量尤其當然需要測試關於其對於發泡操作的影響，如使用量高於0.1重量%之所有另外添加劑。此對於熟習本領域之人士而言不是非常麻煩。
適用之塑化劑、流變改質劑及鏈增長劑在自PEI或包含PEI之摻合物製造片材、膜材或模製品的技術中為一般常識，以及因此可以最小成本及不便轉移以從根據本發明之組成物製造發泡體。
隨意地添加之纖維為用於添加至聚合物組成物的一般已知纖維材料。在本發明之特別適用實施態樣中，纖維為PEI纖維、PES纖維、PPSU纖維或摻合纖維，摻合纖維係選自所提及之聚合物。
例如呈管、小板、棒、球之形式或呈另外的已知形式之奈米粒子通常為無機材料。其可於最終發泡體中同時發揮各種不同功能。此係因為該等粒子在發泡操作中部分作為成核劑之故。該等粒子可進一步影響發泡體之機械性質以及(氣體)擴散性質。該等粒子進一步額外促成低可燃性。
除了所列舉的奈米粒子之外，亦可包括微粒子或大致不溶混之相分離聚合物作為成核劑。在該組成物之成核劑的背景下，所述聚合物必須與另外的成核劑分開觀察，原因係另外的成核劑主要對於發泡體之機械性質、對於組成物之熔體黏度以及因此對於發泡條件發揮影響。作為成核劑之相分離聚合物的額外效果係該組分的額外所希望效果，但並非於該情況下的主要效果。因此，該等額外的聚合物在整體計數中係與其他添加劑分開另外呈現。
隨意地，就添加劑而言亦可能包括多達9重量%之另外的聚合物組分以供調整物理性質。該等額外的聚合物可為例如聚醯胺類、聚烯烴類(特別是PP)、聚酯類(特別是PET)、基於硫之聚合物(例如PSU、PPSU、PES)或聚(甲基)丙烯醯亞胺。
發泡劑之選擇係相對自由的，以及對於熟習本領域之人士而言特別是由所選擇之發泡方法、其於聚合物中之溶解度以及發泡溫度來決定。適用之實例為醇類(例如異丙醇或丁醇)、酮類(諸如丙酮或甲基乙基酮)、烷類(諸如異丁烷、正丁烷、異戊烷、正戊烷、己烷、庚烷或辛烷)、烯類(例如戊烯、己烯、庚烯或辛烯)、CO2 、N2 、水、醚類(例如二乙醚)、醛類(例如甲醛或丙醛)、氫(氯)氟碳化物、化學發泡劑或其二或更多者之混合物。
化學發泡劑係相對或完全非揮發性物質，其係在發泡條件下經歷化學分解以於分解時形成實際發泡劑。三級丁醇為化學發泡劑之非常簡單實例，原因係其於發泡條件下形成異丁烯及水。另外的實例為NaHCO3 、檸檬酸、檸檬酸衍生物、偶氮二甲醯胺(ADC)及/或基於彼之化合物、甲苯磺醯基肼(TSH)、氧雙(苯磺醯肼)(oxybis (benzosulfohydroazide)，OBSH)或5-苯基四唑(5-PT)。
較佳的，根據本發明之粒子發泡體具有大於0.5 MPa的根據ISO1926之抗張強度，介於8%與12%的根據ISO1926之斷裂伸長率，大於8 MPa的根據ASTM C273之於室溫下的剪切模數，大於0.45 MPa的根據ASTM C273之於室溫下的剪切阻力，大於13 MPa的根據ISO 844之於室溫下的壓縮模數，以及大於0.4 MPa的根據ISO 844之於室溫下的抗壓強度。在採用進一步描述之方法用於製造粒子發泡體的情況下，對於熟習本領域之人士而言，依從該等機械性質同時維持根據本發明之玻璃轉化溫度及孔室大小是簡單的事。此外，亦已發現，令人意外的，根據本發明之粒子發泡體可用於滿足根據FAR 25.852之對於用於航空產業中之航空器的內部中特別重要之防火規範或防火性質。
亦非常令人意外的是，如同呈板狀形式之對應發泡體所實現，根據本發明之粒子發泡體實現用於航空器內部中之先決條件所需的全部材料性質。例如就PMI而言，該關係不存在，原因係由板材發泡體所構成之聚甲基丙烯醯亞胺片狀材料滿足該等條件，然而粒子發泡體經常具有比板材發泡體較差之機械性質。已另外發現之特別令人意外的優點係，與板材發泡體相較，該種粒子發泡體無明顯孔室定向(若有任何孔室定向)。此在許多情況下對於粒子發泡體造成有利的各向同性機械性質，然而對應之板材發泡體經常具有在一個區域和與該區域成直角之軸不同的各向異性機械性質。根據特殊用途，各向同性機械性質可能相當有利，尤其是當有來自不同方向的壓應力時。
較佳的，根據本發明之發泡體具有相對於未發泡材料密度降低總計介於1%與98%之間、較佳介於50%與97%之間、更佳介於70%與95%之間的發泡程度。該發泡體較佳具有介於20與1000 kg/m3 之間、較佳介於40與250 kg/m3 之間、尤佳介於50與150 kg/m3 之間的密度。
除根據本發明之粒子發泡體以外，用於製造彼之方法亦為本發明一部分。
原則上，根據本發明，有兩種用於製造PEI粒子發泡體的較佳方法。第一方法變體中，藉由具有穿孔板之擠出機加工由80重量%至99.5重量%之PEI、0.5重量%至10重量%之發泡劑及0重量%至10重量%之添加劑所組成的組成物以產生發泡的或可發泡丸粒。入口區與螺桿尖端之間的溫度較佳係在介於320與400℃之範圍內。此外，在該距離內經常不存在均勻溫度，而是存在例如在聚合物熔體輸送方向中溫度升高之梯度。穿孔板之溫度係介於250與350℃之間，而通過穿孔板離開時之熔體溫度係介於230與360℃之間。裝填發泡劑通常係於擠出機中進行。當水下製粒中之壓力低於發泡劑之膨脹力時，該等丸粒則於其從穿孔板離開時發泡。因而發泡之該等丸粒隨後較佳經進一步加工以產生粒子發泡體。
在該實施態樣之一變體中，可將離開擠出機之組成物導引至水下造粒機中。該水下造粒機係設計成具有防止發泡之溫度及壓力的組合。該製程提供裝載發泡劑之丸粒材料，其於稍後藉由更新供應能量而膨脹至所希望密度及/或藉由隨意的模製進一步加工成珠狀發泡體工件。預發泡必要的能量輸入可藉由接觸式加熱，例如於空氣循環爐中，或藉由IR或微波輻射之基於輻射的方式進行。
在用於製造PEI粒子發泡體之第二方法變體中，最初同樣藉由具有穿孔板之擠出機加工由90重量%至100重量%之PEI及0重量%至10重量%之添加劑所組成的組成物以產生丸粒，但不裝載發泡劑。此處，入口區與螺桿尖端之間的溫度(其同樣不一定均勻)亦在介於320與400℃之範圍內。穿孔板之溫度同樣係介於250與350℃之間，而通過穿孔板離開時之熔體溫度係介於230與360℃之間。此處，該等丸粒隨後於熱壓釜中裝載發泡劑，使該等丸粒含有介於0.5重量%與10重量%之發泡劑。裝載發泡劑之丸粒然後可藉由膨脹及/或藉由加熱至超過200℃之溫度發泡而獲得粒子發泡體。
關於實際發泡，熟習本領域之人士原則上已知將聚合物組成物發泡的各種方法原則上可應用於本組成物，特別是關於用於熱塑性發泡體之方法。例如，該組成物可於介於150與250℃之間的溫度以及介於0.1與2巴之間的壓力下發泡。較佳的，實際發泡若不是跟隨在擠出之後，其係在標準大氣壓下於介於180與230℃之間的溫度下進行。
在稍後裝填發泡劑的變體中，於熱壓釜中在例如介於20與120℃之溫度以及例如介於30與100巴之壓力下將仍無發泡劑之組成物與發泡劑摻混，然後在該熱壓釜內部藉由降低壓力及升高溫度至發泡溫度而膨脹。或者，與發泡劑摻混之組成物係於熱壓釜中冷卻以及於冷卻之後去熱壓(deautoclaved)。該組成物則在日後藉由加熱至發泡溫度而可膨脹。此亦可例如在進一步模製或與其他組件諸如嵌件或面層組合之下發生。
更佳的，不論所使用之方法為何，所製造之粒子發泡體隨後係黏著劑黏接、縫合或熔接至覆蓋材料。此處「熔接」意指加熱組件引起材料之間的內聚或黏著，例如經由在發泡體表面以覆蓋材料部分填充開放式孔達成。
覆蓋材料可包含木材、金屬、裝飾膜、複合材料、預浸材或其他已知材料。
在所使用之材料稍後發泡的情況下，例如，於熱壓釜中裝填發泡劑之後，所製造之粒子發泡體或者亦可於覆蓋材料存在之下發泡，以使其藉由黏著劑黏接或熔接結合至覆蓋材料。
在裝填係於擠出機中進行的方法變體中，PEI或者亦可於離開該擠出機時施加至隨意地含有覆蓋材料之經隨意地加熱之模具中。在該情況下，藉由成形進行發泡以產生粒子發泡體或複合材料。或者，可將離開擠出機之組成物導引至發泡體噴淋裝置。於該裝置中，藉由模製直接發生膨脹。
不論所使用之變體為何，可於發泡期間對粒子發泡體或複合材料提供嵌件，及/或可將通道併入該粒子發泡體中。
根據本發明之發泡體，或藉由根據本發明之方法所製造之發泡體，可用於建造太空船或航空器，尤其是用於其內部或外部。此可包括粒子發泡體，不論是否藉由根據本發明之方法製造，還有由彼實現之複合材料。更特別的，由於本發明之發泡體的低可燃性，該等發泡體亦可安裝於該等載具內部。
更特別的，純PEI粒子發泡體尤其適於併入航空器內部。除了噴射機(jet)或小型航空器以外，航空器尤其包括直升機或甚至太空船。此種航空器內部中之安裝的實例為例如可合攏於客機(passenger aircraft)中之座椅背面之桌板、座椅之填充物、或內部隔板，以及例如用於內部門。
基於含有PEI之摻合物的粒子發泡體另外亦適於併入航空器之外部。「外部」意指不只作為航空器外皮中的填充物，而是尤其亦作為機頭中、機尾區域中、機翼中、外門中、控制表面中或轉子葉片中之填充物。

Claims (13)

  1. 一種PEI粒子發泡體於航空器建造之用途，其特徵在於發泡之PEI的玻璃轉化溫度介於180與215℃之間，以及在於該粒子發泡體的平均孔室直徑(mean cell diameter)小於2 mm。
  2. 如申請專利範圍第1項之粒子發泡體之用途，其中該粒子發泡體已從由80重量%至99.5重量%之PEI、0.5重量%至10重量%之發泡劑以及0重量%至10重量%之添加劑所組成的組成物來獲得。
  3. 如申請專利範圍第1或2項之粒子發泡體之用途，其中該添加劑為阻燃劑、塑化劑、顏料、UV安定劑、成核劑、耐衝擊性改質劑、黏著促進劑、流性改質劑、鏈增長劑、纖維及/或奈米粒子。
  4. 如申請專利範圍第1至3項中至少一項之粒子發泡體之用途，其中該發泡劑包含醇、酮、烷、烯、CO2 、N2 、水、醚、醛、化學發泡劑或其二或更多者之混合物。
  5. 如申請專利範圍第1至4項中至少一項之粒子發泡體之用途，其中該粒子發泡體具有大於0.5 MPa的根據ISO1926之抗張強度，介於8%與12%的根據ISO1926之斷裂伸長率，大於8 MPa的根據ASTM C273之於室溫下的剪切模數，大於0.45 MPa的根據ASTM C273之於室溫下的剪切阻力，大於13 MPa的根據ISO 844之於室溫下的壓縮模數，以及大於0.4 MPa的根據ISO 844之於室溫下的抗壓強度。
  6. 如申請專利範圍第1至5項中至少一項之粒子發泡體之用途，其中該粒子發泡體已安置於航空器內部。
  7. 如申請專利範圍第1至6項中至少一項之粒子發泡體之用途，其中該粒子發泡體之平均孔室直徑小於500 μm。
  8. 一種用於製造針對如申請專利範圍第1至7項中至少一項之用途的PEI粒子發泡體之方法，其特徵在於藉由具有穿孔板之擠出機加工由80重量%至99.5重量%之PEI、0.5重量%至10重量%之發泡劑以及0重量%至10重量%之添加劑所組成的組成物以產生發泡之丸粒，其中在入口區與螺桿尖端之間的溫度係在介於180與380℃之範圍內，該穿孔板之溫度係在介於250與350℃，以及通過該穿孔板之出口的熔體溫度係介於230與360℃；以及在於該等發泡之丸粒隨後發泡以進一步產生粒子發泡體。
  9. 一種用於製造針對如申請專利範圍第1至7項中至少一項之用途的PEI粒子發泡體之方法，其特徵在於藉由具有穿孔板之擠出機加工由90重量%至100重量%之PEI及0重量%至10重量%之添加劑所組成的組成物以產生丸粒，其中在入口區與螺桿尖端之間的溫度係在介於180與380℃之範圍內，該穿孔板之溫度係在介於300與350℃，以及通過該穿孔板之出口的熔體溫度係介於250與360℃；在於該等丸粒隨後係於熱壓釜中承載(laden)發泡劑使彼等含有介於0.5重量%與10重量%之間的發泡劑；以及在於然後藉由膨脹及/或藉由加熱至超過200℃之溫度使該等承載發泡劑的丸粒發泡以產生粒子發泡體。
  10. 一種用於製造複合部件之方法，其特徵在於藉由如申請專利範圍第8或9項之方法所製造的該粒子發泡體係經黏接、縫合或熔接至覆蓋材料。
  11. 一種用於製造複合部件之方法，其特徵在於藉由如申請專利範圍第8或9項之方法所製造的該粒子發泡體係於覆蓋材料的存在下發泡，使其藉由黏著劑黏接或熔接而結合至該覆蓋材料。
  12. 如申請專利範圍第8項之方法，其中將在離開該擠出機之出口的PEI引入隨意地含有覆蓋材料之經隨意地加熱之模具中，且發泡成形以產生粒子發泡體或複合材料。
  13. 如申請專利範圍第8至12項中至少一項之方法，其中於發泡期間將嵌件及/或通道併入該粒子發泡體。
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