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TW201641529A - 用於製造ｐｕｒ發泡體的聚醇組份 - Google Patents

用於製造ｐｕｒ發泡體的聚醇組份 Download PDF

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Publication number
TW201641529A
TW201641529A TW105107524A TW105107524A TW201641529A TW 201641529 A TW201641529 A TW 201641529A TW 105107524 A TW105107524 A TW 105107524A TW 105107524 A TW105107524 A TW 105107524A TW 201641529 A TW201641529 A TW 201641529A
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Taiwan
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polyol
composition
component
composition according
pur foam
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TW105107524A
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English (en)
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TWI706967B (zh
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克里斯鈞 貝瑟爾
丹尼爾 巴爾
席林 查塔德
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杭斯曼高級材料公司
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Abstract

本發明係關於一種組成物，其包含：(a1)聚醚聚醇，(a2)聚烯烴聚醇及(a3)可藉由環氧化不飽和脂肪酸酯且隨後與含有活性氫之化合物進行開環反應獲得的聚酯聚醇，其可用於製備藉由低溫可撓性及低介電損耗區分的PUR發泡體，且適合於在製造浸樹脂紙(RIP)套管中填充電容器芯體與外部複合物或瓷絕緣體之間的間隙。

Description

用於製造PUR發泡體的聚醇組份
本發明係關於聚醇組成物，其與適合之聚異氰酸酯組合提供聚胺甲酸酯(polyurethane；PUR)發泡體，該等發泡體可在製造高電壓(high voltage；HV)浸樹脂紙(resin impregnated paper；RIP)套管期間有利地施用以填充電容器芯體與外部中空絕緣體(複合物類型或瓷)之間的間隙。
RIP電容器芯體藉由使用在插入鋁箔的同時連續捲繞之褶皺紙來製造以建立電容分級之電場強度。在捲繞製程之後，芯體在真空及熱下用環氧樹脂浸漬。之後機器加工實心芯體以完成最終尺寸。典型地，RIP套管具有外部複合物或瓷絕緣體，且在電容器芯體與外部複合物或瓷絕緣體之間的間隙用發泡體，通常PUR發泡體填充。
由可適當地用作用於RIP套管之填充材料的PUR發泡體滿足之要求為多方面的。
可發泡組成物通常由兩種組份(聚醇組份及聚異氰酸酯組份)組成，其在應用之前不久，亦即在生成PUR發泡體之前不久混合。由於聚醇組份常含有數種聚醇以及各種(分散)添加劑，所以此等混合物經常傾向於沉澱固體組份或分離。因此，聚醇組份之儲存穩定性為重要因素。
另外，可發泡組成物應確保足夠長的適用期，以允許填充較 大超高電壓(ultra-high voltage，UV)套管，亦即在混合組份之後，組成物之黏度應僅適度地增加。適用期通常按照自合併聚醇及異氰酸酯組份(包括添加劑)起直至黏度增加至15Pa‧s的時間段來指定，且對於預期用途應為>90分鐘。
為了耐受較大溫度差異，需要固化PUR發泡體展現實質性低溫可撓性。因此，玻璃轉移溫度Tg應相當低：Tg<-50℃。
用於HV套管的絕緣材料最重要的為介電性質。因此，介電損耗的目標分別為tan δ<5%(RT)及tan δ<15%(100℃)。
US 4,752,626描述一種在寬範圍異氰酸酯指數下具有較低壓縮永久變形的高彈性胺甲酸酯發泡體，其用於整體式發泡體零件中之小空隙填充。
整體式發泡體零件之模製製程中形成的小空隙可在不使發泡液體滲透至現存發泡體單元中之情況下填充。另外，所得發泡體在寬範圍異氰酸酯指數下具有極低壓縮永久變形值。
根據US 4,752,626之發泡系統由搖變減黏聚異氰酸酯組份及搖變減黏聚醇組份構成，該搖變減黏聚醇組份為重量比在95/5至50/50之間的聚烯烴聚醇及聚氧伸烷基聚醇之摻合物。搖變減黏性藉由將苯亞甲基山梨糖醇添加至各別組份來獲得。儘管此PUR發泡體非常適用於填充在汽車發泡體零件之模製製程中形成的小空隙，但應用於HV電容器在適用期、低溫可撓性及電氣效能方面要求更為嚴格。
本發明之目標為提供由儲存穩定的聚醇組份及聚異氰酸酯 組份組成的可發泡組成物，其確保足夠長的適用期、低溫可撓性、低介電損耗及在固化期間令人滿意的組份相容性。
目前已發現此等性質可藉由使用作為聚醇組份之特定組成物(A)來實現，該組成物包含(a1)聚醚聚醇，(a2)羥基封端之聚丁二烯或聚異戊二烯及(a3)可藉由環氧化不飽和脂肪酸酯且隨後與含有活性氫之化合物進行開環反應獲得的聚酯聚醇。
作為組份(a1)之聚醚聚醇可例如藉由起始物與環氧烷，例如與環氧乙烷、環氧丙烷或環氧丁烷或四氫呋喃反應來獲得。起始物在此為通常適合於製備具有2或3之官能度之聚醚聚醇的所有起始物，例如水、脂族、環脂族或芳族聚羥基化合物(具有2或3個羥基)，諸如乙二醇、丙二醇、丁二醇、己二醇、辛二醇、二羥基苯或雙酚(例如雙酚A)、三羥甲基丙烷或胺(參看Ullmanns Encyclopädie der Technischen Chemie(Ullmann's Encyclopedia of Industrial Chemistry)，第4版，第19卷，Verlag Chemie GmbH,Weinheim 1980，第31頁至第38頁，第304頁及第305頁)。
尤其適合作為根據本發明之組成物成分(a1)的物質為基於環氧乙烷之聚醚-聚醇及基於環氧丙烷之聚醚-聚醇，以及可為無規或嵌段共聚物的對應環氧乙烷/環氧丙烷共聚物。在此等共聚物中環氧乙烷與環氧丙烷之比率可在較寬界限內改變。因此，舉例而言，僅聚醚-聚醇之末端羥基可能與環氧乙烷反應(末端遮蔽)。
基於聚乙烯及/或聚丙烯之聚醚-聚醇的分子量Mw較佳為100 至2000g/mol、更佳地200至1000g/mol且尤其300至600g/mol。
亦應指出，比如上文已定義之聚伸烷基二醇，聚四氫呋喃(例如由LyondellBasell供應之POLYMEG®)同樣為商業上可獲得的。
較佳地，線性或分枝聚環氧乙烷或聚環氧丙烷在根據本發明之組成物中用作組份(a1)。
羥基封端之環氧乙烷/環氧丙烷嵌段共聚物尤其較佳作為組份(a1)。
根據組份(a2)之聚烯烴聚醇為已知的且在一定程度上為商業上可獲得的。聚烯烴聚醇之聚合物主鏈典型地為烯烴單體之聚合產物或烯烴單體與芳乙烯單體之聚合產物。烯烴單體宜含有2至12個碳原子。較佳地，烯烴單體為具有4至10個碳原子，更佳地4至6個碳原子之二烯。
最佳烯烴單體為丁二烯及異戊二烯，特定言之1,3-丁二烯。
可與烯烴單體共聚的芳乙烯單體較佳為單芳乙烯單體，比如苯乙烯或烷基取代之苯乙烯。根據組份(a2)之聚烯烴聚醇可含有至多50重量%經聚合的芳乙烯單體，例如0.01至20.0重量%且尤其0至5重量%。
在一較佳具體實例中，根據組份(a2)之聚烯烴聚醇不含有任何聚合芳乙烯單體。
根據本發明之適合聚烯烴聚醇亦可完全或部分為烯烴單體之經氫化聚合產物或烯烴單體與芳乙烯單體之經氫化聚合產物。聚合物之氫化可根據已知方法處理，例如藉由在催化劑，比如美國專利5,039,755中所述之雷氏(Raney)鎳、鉑、鈀或可溶過渡金屬催化劑及鈦催化劑存在下的氫化進行。
若聚烯烴聚醇衍生自1,3-丁二烯，則聚丁二烯較佳地由至少15%之1,2-加成產物組成。
若聚烯烴聚醇衍生自異戊二烯，則聚異戊二烯較佳地由至少80%之1,4-加成產物組成。
聚烯烴聚醇的分子量Mn(數目平均值，藉由凝膠滲透層析術(GPC)量測)較佳地為500至20000、更佳地1000至15000且尤其較佳2000至5000。
聚烯烴聚醇較佳展現的官能度為1.5至3.0個羥基/分子，更佳地1.8至2.6個羥基/分子且尤其1.9至2.5個羥基/分子。
聚烯烴聚醇較佳為聚二烯二醇，尤其聚-1,3-丁二烯二醇。
適合之聚-1,3-丁二烯二醇為下式化合物， 其中x、y、z、v及w表示結構單元之百分比，且指示以下範圍：x=10-70%，y=15-70%，z=10-30%，v=10-75%， w=25-90%，其限制條件為x+y+z=100%及v+w=100%。
根據式(1)及(2)之聚烯烴聚醇為市售的，例如Poly bd® R45 HTLO(由CRAY VALLEY供應)。
所主張組成物之根據組份(a3)之聚酯聚醇為同樣已知的，且描述於例如Polymer Reviews 52(1),38-79(2012)中。製備該等聚酯聚醇之起始產物為主要由三酸甘油酯組成的植物油，其中甘油之三個羥基已用脂肪酸酯化。此等脂肪酸可為飽和的，亦即含有非反應性脂族鏈(比如硬脂酸或棕櫚酸)，或不飽和的，亦即含有攜帶雙鍵之脂族鏈(比如油酸、亞麻油酸、次亞麻油酸或蓖麻油酸)。然而，三酸甘油酯必需含有至少兩個雙鍵。植物油可根據本身已知之方法，例如利用與由乙酸及過氧化氫之反應原位形成的過氧乙酸反應來環氧化。其他適合之方法為植物油之酶促環氧化或藉由微波來環氧化。
環氧化物之開環反應可在酸性催化劑，比如硫酸、對甲苯磺酸、氟硼酸、過氯酸或氟銻酸存在下與各種氫活性化合物Nu-H進行，其中Nu指示羥基、胺基、烷基胺基、羥基烷胺基、二烷基胺基、二(羥基烷基)胺基、烷氧基、羥基烷氧基、烷硫基或烷醯氧基。
以此方式，可製備在分子量、黏度及官能度方面突出的各種聚酯聚醇。
較佳的聚酯聚醇展現2至4個、特定言之2.5至3.5個官能度(每分子羥基數)；100至300、特定言之150至250之中位羥值；200至500、特定言之300至400之中位羥基當量；及100至2500mPa‧s、特定言 之200至500mPa‧s之中位黏度(25℃)。
此類型之聚酯聚醇為市售的，例如商品名稱為SOVERMOL®，由BASF供應。
作為組份(a3)尤其較佳的為SOVERMOL® 1111，其為具有3.0之官能度、160之中位羥值、350之中位羥基當量及500mPa‧s之中位黏度(25℃)的分枝聚酯聚醇。
根據本發明之聚醇組份(A)可包含其他適合於PUR技術的慣用添加劑，例如催化劑、表面活性物質、乾燥劑、填充劑、染料、顏料、防焰劑、軟化劑、熱老化穩定劑、搖變減黏劑、起泡劑及發泡體穩定劑，例如聚矽氧及二羧酸。
適合之催化劑為例如三級胺(諸如N-甲基二乙醇胺、三乙醇胺、二苯基甲基胺或二氮雜二環辛烷)或有機錫化合物(諸如月桂酸二丁基錫)。
作為用於PUR發泡體的防焰劑，通常應用磷化合物(比如磷酸三甲苯酯或二甲基甲烷膦酸酯)或含鹵素之聚醇。亦可使用無機阻燃劑，比如水合氧化鋁、三氧化二銻及多磷酸銨。
礦物油可作為軟化劑添加。適合之產物為例如在商品名稱NYFLEX®下市售的油(由Nynas供應)。
用於根據本發明之聚醇組份的適合之熱老化穩定劑為例如脂族縮水甘油醚，比如聚丙二醇二縮水甘油醚。
較佳搖變減黏劑為熔融矽石，例如在商品名稱AEROSIL®下市售的產物(由Evonik供應)。
在根據本發明之聚醇組份中添加劑之總含量以所有組成物計宜為0至30重量%、較佳地0至15重量%。
在極低反應性(凝膠時間>2h)之情況下，極推薦添加特定發泡體穩定劑。
因此，本發明之另一具體實例為含有如上所定義組份(a1)、(a2)及(a3)及另外(a4)聚矽氧烷-聚氧伸烷基嵌段共聚物的聚醇組份(A)。
聚矽氧烷-聚氧伸烷基嵌段共聚物作為用於PUR發泡體的穩定劑描述於例如US-A 6,166,098及EP-A 936 240中，且例如在商標名稱TEGOSTAB®(由Evonik供應)及DABCO®(由Air Products供應)下市售。
穩定劑TEGOSTAB® B 8863 Z為尤其較佳的。
用於聚醇組份(A)的組份(a1)、(a2)及(a3)以及視情況選用之(a4)之量可在寬界限內改變。
以所有組成物(包括添加劑)之重量計，包含以下各者之組成物，(a1)5至30重量%、較佳地7至20重量%、尤其8至15重量%之聚醚聚醇，(a2)30至70重量%、較佳地35至65重量%、尤其40至60重量%之羥基封端之聚丁二烯或聚異戊二烯及(a3)10至50重量%、較佳地12至40重量%、尤其15至30重量%之聚酯聚醇，其可藉由環氧化不飽和脂肪酸酯且隨後與含有活性氫之化合物進行開環反應獲得， 已證明為有利的。
在製備PUR發泡體中，含有包含組份(a1)、(a2)及(a3)之組成物的聚醇組份(A)與聚異氰酸酯反應。適用於製備根據本發明之PUR發泡體的聚異氰酸酯亦在此項技術中熟知，且為每分子含有至少兩個異氰酸酯基團的有機化合物。可採用任何該等化合物或其混合物。異氰酸酯可為芳族、環脂族或脂族，且可為單體或寡聚化合物。
本發明因此進一步關於含有以下之組成物(A)包含如申請專利範圍第1項之組份(a1)、(a2)及(a3)的組成物及(B)聚異氰酸酯。
用於適合之聚異氰酸酯的特定實例為十二烷-1,12-二異氰酸酯、2-乙基四亞甲基-1,4-二異氰酸酯、2-甲基五亞甲基-1,5-二異氰酸酯、四亞甲基-1,4-二異氰酸酯、六亞甲基-1,6-二異氰酸酯、環己烷-1,3-二異氰酸酯、環己烷-1,4-二異氰酸酯、異佛爾酮二異氰酸酯、六氫甲苯-2,4-二異氰酸酯、六氫甲苯-2,5-二異氰酸酯、二環己基甲烷-2,2'-二異氰酸酯、二環己基甲烷-4,4'-二異氰酸酯、二環己基甲烷-2,4'-二異氰酸酯、甲苯-2,4-二異氰酸酯、甲苯-2,6-二異氰酸酯、二苯基甲烷-2,2'-二異氰酸酯(2,2'-MDI)、二苯基甲烷-4,4'-二異氰酸酯(4,4'-MDI)、二苯基甲烷-2,4'-二異氰酸酯(2,4'-MDI)及聚苯基聚亞甲基聚異氰酸酯(粗MDI)。
有機二異氰酸酯及聚異氰酸酯可個別地或以其混合物形式使用。
市售二異氰酸酯經常含有二聚(脲二酮)、三聚(三)及寡聚 化合物。在根據本發明之組成物中，單體及寡聚物之此等混合物可在不分離副產物或純化之情況下採用。
較佳二苯基甲烷二異氰酸酯、更佳地二苯基甲烷-4,4'-二異氰酸酯或二苯基甲烷-2,4'-二異氰酸酯用於根據本發明之發泡體。
在本發明之一尤其較佳具體實例中，將約60%4,4'-亞甲基二苯基二異氰酸酯、約20%2,4'亞甲基二苯基二異氰酸酯及約20%聚合亞甲基二苯基二異氰酸酯之混合物作為異氰酸酯組份(B)應用。
自根據本發明之組份(A)及(B)製備的發泡或不發泡PUR展現出色的性質，且可用於各種應用，較佳地作為絕緣材料用於電工技術。
本發明因此關於含有如上所定義組份(A)及(B)之組成物之用途，其作為用於電組件的囊封材料。
為了製備根據本發明之PUR發泡體，組份(A)及(B)以組份(B)之NCO基團與組份(a1)、(a2)及(a3)之反應性氫原子總和的當量比率為(0.85-1.75)：1、較佳地(1.0-1.3)：1的該等量反應。若基於異氰酸酯之發泡體含有至少一些鍵結之異氰尿酸酯基團，則通常採用的該等組份之比率為(1.5-60)：1、較佳地(3-8)：1。
一般而言，發泡劑在PUR形成反應期間提供。發泡劑可為空氣、氮氣、二氧化碳或任何其他惰性氣體。發泡劑亦可為水(其與異氰酸酯反應，生成原位二氧化碳)或氟化烴，諸如二氯二氟甲烷、1,1-二氯-1-氟乙烷、1-氯-1,1-二氟乙烷、2,2-二氯乙烷或其類似物。諸如戊烷及丙酮之非氟化有機化合物亦可用作起泡劑。所需發泡劑之量將根據所需發泡體之密度改變。適合含量之起泡劑對技術人員為已知的。
本發明進一步關於利用上文所述之方法製備的PUR發泡體之用途，其在製造浸樹脂紙(RIP)套管中用於填充電容器芯體與外部複合物或瓷絕緣體之間的間隙。
根據本發明之PUR發泡體的另一潛在應用領域為曝露於極限溫度及壓力的管道之熱隔離，例如用於深海中開採油及氣體沉積物的管道。
因此，本發明進一步關於利用上文所述之方法製備的PUR發泡體之用途，其作為用於管道的絕緣材料。
另外，利用本發明方法製備的PUR發泡體可有利地作為填充材料應用於空心複合物絕緣體中。
因此，利用上文所述之方法製備的PUR發泡體在製造空心複合物絕緣體中用於填充空心管中的空間為本發明之另一目標。
藉由以下非限制性實施例說明本發明。
實施例
所用原材料之清單
BAYGAL ® K 55(由Bayer供應)：無色至黃色三官能聚環氧丙烷/聚環氧乙烷嵌段共聚物；黏度：約600mPas；羥值：370至400mg KOH/g。
TEGOSTAB ® B 8863 Z(由Evonik供應)： 聚醚改質之聚矽氧烷，推薦作為用於PUR發泡體的發泡體穩定劑；LUPRANOL ® 2095(由BASF供應)：具有一級羥基端基的三官能聚醚聚醇；推薦用於製備彈性發泡體材料；黏度：約850mPas；羥值：35mg KOH/g(DIN 53 240)；ARALDITE ® DY 3601(由Huntsman供應)：聚丙二醇二縮水甘油醚，環氧化物數目：2.47至2.60eq/kg(ISO 3001)；NYFLEX 820(由Nynas GmbH供應)：來自石油的液體環烷烴，黏度：在40℃下90至110cSt(ASTM 445)；Poly bd ® R45 HTLO(由CRAY VALLEY供應)：液體羥基封端之聚丁二烯，黏度：在30℃下5Pas，羥基官能團：2.5，分子量Mn：2800g/mol，1,2乙烯基含量：20%；SOVERMOL ® 1111(由BASF供應)：分枝聚醚酯，黏度：在25℃下300至700mPas(DIN 53015)；UOPL膏(由UOP供應)大致孔徑為3Å之沸石A類型的鋁矽酸鉀鈣鈉於蓖麻油中之50%膏；AEROSIL ® 200(由Evonik供應)比表面積為200m2/g的親水性煙霧狀二氧化矽；SUPRASEC ® 2447(由Huntsman供應)：含有約60%4,4'-亞甲基二苯基-二異氰酸酯、約20%2,4'-亞甲基二苯基-二異氰酸酯及約20%聚合亞甲基二苯基二異氰酸酯的異氰酸酯摻合物；
組份A之製備
製備用於根據本發明之實施例1至3(實施例1至實施例3) 及參考實施例1至3(C1至C3)的組份A：將根據表1之各調配物的所有組份(除SUPRASEC® 2447外)以給定比例放入至具有足夠尺寸的金屬罐中，產生200g聚醇混合物。混合物接著藉由在23℃下用螺旋槳攪拌器攪拌組份約2分鐘以產生組份A來製備。
組份B之製備：
作為用於根據本發明之實施例1至3(實施例1至實施例3)及參考實施例1至3(C1至C3)的組份B，使用100%Huntsman之SUPRASEC® 2447。
組份A及B之反應性混合物的製備：
將根據表1之約150g組份A及對應量之組份B放入至金屬罐中，且接著在環境溫度下用螺旋槳攪拌器混合2分鐘。接著將80g此反應性混合物隨後用於製備發泡體，且重置以製備用於如以下中所述tan δ測試的板。結果概括於表1中。
發泡體之製備及發泡體穩定性判斷：
將80g聚醇/異氰酸酯混合物放入至200ml杯中，且接著用小型高剪切分散器混合器以2000rpm攪拌30秒。此設備具有的此剪切足以將由於發泡體形成而獲得約30%體積增加的該空氣之量引入。所生成發泡體接著在23℃下固化72小時。固化發泡體樣品之態樣接著檢查其均質性。通過此發泡體穩定性測試的要求為沒有展示塌陷跡象。
判斷聚醇混合物之儲存穩定性：
需要聚醇混合物(組份A)在室溫下經1個月之時段明確保持無分離跡象。展示組份之不相容性的調配物在一段時間之後通常顯示超 過1個相。
黏度量測：
組份A及B之混合物經受Rheomat黏度計，且登記黏度之進展直至達到15Pas。記錄達至15Pas所需時間。黏度根據DIN 53019量測。
Tan δ及T g 量測：
組份A及B之混合物澆鑄(在無發泡之情況下)至模具中，且1及2mm厚的板藉由在90℃下固化混合物4小時製備。Tan δ接著在2mm厚的板上根據IEC 60250量測。
Tg藉由DMA在1mm厚的板上根據IEC 6721-2量測。
根據實施例1至3之組成物提供長適用期、低Tg(良好低溫可撓性)、低tan δ(良好電氣效能)及高儲存穩定性之組合，而根據參考實施例1至3(C1至C3)之組成物沒有達成<-50℃之目標低Tg以及<5%(RT)及<15%(100℃)之所需低tan δ。

Claims (14)

  1. 一種組成物，其包含(a1)聚醚聚醇，(a2)聚烯烴聚醇及(a3)可藉由環氧化不飽和脂肪酸酯且隨後與含有活性氫之化合物進行開環反應獲得的聚酯聚醇。
  2. 如申請專利範圍第1項之組成物，其包含作為組份(a1)的線性或分枝聚環氧乙烷或聚環氧丙烷。
  3. 如申請專利範圍第1項之組成物，其包含作為組份(a1)的羥基封端之環氧乙烷/環氧丙烷嵌段共聚物。
  4. 如前述申請專利範圍中任一項之組成物，其包含作為組份(a2)的聚-1,3-丁二烯聚醇或聚異戊二烯聚醇。
  5. 如前述申請專利範圍中任一項之組成物，其包含作為組份(a3)的可自作為不飽和脂肪酸酯之植物油獲得的聚酯聚醇。
  6. 如前述申請專利範圍中任一項之組成物，其另外含有(a4)聚矽氧烷-聚氧伸烷基嵌段共聚物。
  7. 如申請專利範圍第1項之組成物，其包含，以該所有組成物之重量計，(a1)5至30重量%之聚醚聚醇，(a2)30至70重量%之羥基封端之聚丁二烯或聚異戊二烯及(a3)10至50重量%之聚酯聚醇，其可藉由環氧化不飽和脂肪酸酯且隨後與含有活性氫之化合物進行開環反應獲得。
  8. 一種組成物，其含有 (A)包含如申請專利範圍第1項之組份(a1)、(a2)及(a3)的組成物及(B)聚異氰酸酯。
  9. 如申請專利範圍第8項之組成物，其含有作為組份B的二苯基甲烷二異氰酸酯。
  10. 一種如申請專利範圍第8項之組成物之用途，其作為用於電組件的囊封材料。
  11. 一種用於製備PUR發泡體之方法，其藉由使(A)含有如申請專利範圍第1項之組成物的聚醇組份與(B)聚異氰酸酯在起泡劑存在下反應。
  12. 一種如申請專利範圍第11項之方法製備的PUR發泡體之用途，其在製造浸樹脂紙(RIP)套管中用於填充在電容器芯體與外部複合物絕緣體之間的間隙。
  13. 一種如申請專利範圍第11項之方法製備的PUR發泡體之用途，其作為用於管道的絕緣材料。
  14. 一種如申請專利範圍第11項之方法製備的PUR發泡體的用途，其在製造空心複合物絕緣體中用於填充該空心管中的空間。
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