TW201806726A - 經由使用增加導熱性的添加劑來縮短聚合物粒子發泡的冷卻期 - Google Patents

經由使用增加導熱性的添加劑來縮短聚合物粒子發泡的冷卻期 Download PDF

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Publication number
TW201806726A
TW201806726A TW106110176A TW106110176A TW201806726A TW 201806726 A TW201806726 A TW 201806726A TW 106110176 A TW106110176 A TW 106110176A TW 106110176 A TW106110176 A TW 106110176A TW 201806726 A TW201806726 A TW 201806726A
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Taiwan
Prior art keywords
foaming
polymer particles
particles
mold
expanded
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TW106110176A
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English (en)
Inventor
凱 柏恩哈德
伊娜 雷柏
莫納 拉佩爾
克利斯汀 特瑞瑟
湯瑪斯 理查特
弗羅里恩 貝克
丹尼斯 霍林
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贏創羅恩有限責任公司
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Publication of TW201806726A publication Critical patent/TW201806726A/zh

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Abstract

本發明係關於聚合物粒子，特別是聚(甲基)丙烯醯亞胺(P(M)I)粒子的發泡方法，該粒子可進一步加工以提供發泡模塑物或複合物件。此方法的特點在於聚合物細粒包含改良發泡時的導熱性之填料。該細粒可以例如在最終發泡期間內在壓縮模具中模製以提供具發泡芯的模塑物或複合工件。

Description

經由使用增加導熱性的添加劑來縮短聚合物粒子發泡的冷卻期
本發明係關於聚合物粒子，特別是聚(甲基)丙烯醯亞胺(P(M)I)粒子的發泡方法，該粒子可進一步加工以提供發泡模塑物或複合物件。此方法的特點在於包含改良導熱性的填料之聚合物細粒經發泡。該細粒可以例如在最終發泡期間內在壓縮模具中模製以提供具發泡芯的模塑物或複合工件。
聚合物粒子，特別是P(M)I粒子，在密閉模具中之發泡藉長的加工時間達成，此特別是因為自模具移除之前須要冷卻時間之故。根據本發明減少該時間的方式在於在發泡之後，憑藉在發泡方法中，存在於粒子中的填料更迅速地冷卻模具。
DE 27 26 260描述於高溫仍保留極佳的機械性質之聚(甲基)丙烯醯亞胺發泡體(P(M)I發泡體)之製造。該發泡體係藉鑄塑法製造，即，單體和所須的其他 物質混合及在模具腔中聚合。該聚合物係藉由在第二步驟中加熱而發泡。這些方法非常複雜且難自動化。這些鑄塑方法仍是最為相關的先前技術，特別是用於P(M)I發泡體。但是，只有在發泡完成時才可能進行此類型的發泡體之成型以得到片材。此類型的方法因此極為複雜且費時，特別是用於具有相對的高複雜性的形狀之時。
除了PMI發泡體以外，也有其他基於甲基丙烯酸和丙烯腈的已知發泡體(PI發泡體)具有類似的性質。這些述於例如CN 100420702C。但是，這些發泡體大多也是經由片型聚合反應(sheet polymerization)製得。
除了這些始於未發泡的聚合物片的方法以外，也已經知道始於細粒的“模具內發泡”方法。但是，基本上，相較於上述方法，這些具有數個缺點：得到不均勻的孔結構，原始粒子內部之間和介於原始粒子之間的邊緣展現差異。此外，更觀察到，在發泡期間內，在介於原始粒子之間形成的邊緣處，自細粒發泡的這些產物的黏合性相對欠佳，並因此而使得機械性質不及自半完成的片發泡的材料。
WO 2013/05947描述一種模具內方法，其中至少解決較後提到的問題，其方式在於，在粒子引至成型和發泡模具之前，其經黏著促進劑塗覆，例如經聚醯胺或聚甲基丙烯酸酯塗覆。因此達到晶粒邊緣之極佳的黏著性。但是，此方法未消除最終產物中之不均勻的孔分佈的問題。
WO 2014/076333描述一種方法，其中P(M)I粒子先預發泡才引至用於最終發泡的模具以得到最終工件。相較於其他的模具內發泡方法，此種改良得到較佳的密度分佈和較低的缺陷率。
但是，所有的這些模具內發泡方法仍須要相對長的加工時間。此特別歸因於在最終發泡之後，在模具內之相對長的冷卻階段。
鑑於所討論的先前技術，因此，本發明的目的是提出新穎的模具內發泡方法，其可以簡單的方式和高產製速率提供P(M)I粒子。相較於已知方法，此方法的目標特徵為提高速率和節能。
本發明的另一目的係提供，用於模具內發泡，P(M)I材料，其中該材料的發泡/最終發泡可以在習知之用於模具內發泡的模具內進行。
一個特別的目的在於本發明方法的發泡後模具內冷卻階段比先前技術的方法特別短。
先前技術、討論、申請專利範圍或本發明之實例可衍生出此處未明確討論的其他問題。
下文中，“聚(甲基)丙烯醯亞胺”是指聚甲基丙烯醯亞胺、聚丙烯醯亞胺和其混合物。對應的考量亦 應用於對應的單體，例如(甲基)丙烯醯亞胺和(甲基)丙烯酸：例如，(甲基)丙烯酸是指甲基丙烯酸或丙烯酸或此二者之混合物。
經由用於製造發泡體(例如聚(甲基)丙烯醯亞胺發泡體)之新穎的模具內發泡方法達到目的。此方法的特徵在於聚合物粒子或預發泡的聚合物粒子a)被引至模具，b)於發泡溫度T1發泡，c)冷卻，和d)於移除溫度T2下移除最終的發泡體部件。本發明方法的特徵在於聚合物粒子包含基質材料、至少一種起泡劑和導熱性填料。
較佳地，該基質材料是聚甲基丙烯醯亞胺(PMI)、聚丙烯醯亞胺(PI)、聚丙烯(PP)、聚胺甲酸酯(PU)或聚氯乙烯(PVC)。較佳者是PMI或PI。
該導熱性填料較佳地為鋁、銀、銅、鎂、碳纖維、氧化鋁、氮化鋁、碳化矽、氮化硼或這些的混合物。該填料較佳地為粉末、球、小板、薄片或長粒的形式。此處，在填料上可測得的最大直徑較佳地由100μm至5mm，特別佳地由150μm至2mm。
該起泡劑較佳地為醇、烷、烯、酮、醛或這些的混合物。該起泡劑於標準壓力的沸點是35至150℃。藉由對照所用的基質材料和發泡條件，嫻於此技術者得以輕易地準確選擇起泡劑：亦可能添加CO2而發泡。
本發明的聚合物粒子有各種具體實施例：導熱性填料至少某些程度地位於該聚合物粒子內。此類型的 具體實施例中，較佳地，導熱性填料完全埋在基質材料內。
本發明的第二具體實施例中，發泡性的導熱性填料之位置介於個別聚合物粒子之間。此具體實施例中，較佳地，該導熱性填料至少某些程度地位於該聚合物粒子的表面上。在特別的變體中，聚合物粒子經黏著促進劑塗覆，或者有細粒黏著促進劑存在於個別聚合物粒子之間。在此類型的變體中，更可能地，導熱性填料埋在黏著促進劑內。
此處將上述各種具體實施例或變體之組合視為本發明的其他具體實施例：導熱性填料可以某些程度地位於聚合物粒子內及某些程度地介於其間或在其表面上。
本發明之特別的具體實施例中，該起泡劑是包含至少一種在發泡條件下經由化學反應釋出揮發性化合物的起泡劑之混合物。此類型的起泡劑特別選自下列者：共聚至基質材料中的三級丁醇、異丙醇、或(甲基)丙烯酸異丙酯或(甲基)丙烯酸三級丁酯。
較佳地，發泡溫度T1是由120至300℃，特別是由150至280℃。確實的發泡溫度取決於所用的基質材料和起泡劑。
本發明之特別的具體實施例中，未發泡的聚合物粒子藉使用紅外射線預發泡，該紅外射線之至少80%的波長是由1.4至10.0μm，特別佳地由5.3至6.5μm或由7.8至8.9μm，之後才將該預發泡的粒子引至模具。未 經預發泡之聚合物粒子的尺寸是由0.5至5.0mm。
一個較佳的具體實施例中，本發明之方法之進行方式是使得未經預發泡的P(M)I粒子被置於運輸裝置，例如傳輸帶上，且運送通過具有特別發射所欲波長範圍之適當IR射線源的加熱單元。為得到特別良好的結果，裝載此運輸裝置的方式是使得P(M)I粒子在其上形成單層且全數直接受熱，例如經IR射線源照射。此預發泡較佳地僅進行5分鐘，特別佳地進行3分鐘。此處用於所述具體實施例的預發泡時間與粒子尺寸、起泡劑類型和起泡劑濃度、射線源的波長、與射線源的距離和射線強度有關。用於粒子的運送速率之設定因而與預發泡時間有關。
較佳地，發泡期間至多2分鐘。特別地，步驟a)至d)共進行3至30分鐘。此極短的加工時間，和藉此可能造就高的產製速率，亦被視為本發明的重大優點。
已證實特別有利地，在步驟a)中，粒子被抽吸和/或吹入模具中。藉此，模具中粒子的充填高度為50至100%。
本發明之模具較佳地為成型模具。這些成型模具有數種變體，其中的一個可能性係使用模具內發泡以將實際的發泡材料成型。此類型的下游方法可見於例如EP 2 598 304。另一可能性是不僅模製發泡體，同時亦在其外部提供材料，例如複合材料。因此，易自本發明之預發泡的P(M)I粒子製造形狀複雜的發泡體-芯複合材料。
也可以使用黏著促進劑以改良介於發泡體芯材和外層之間的黏著性，該黏著性在製造複合材料的後續步驟中具重要性。另一可能性在於代替在後續步驟中施用，這些黏著促進劑亦可以在本發明的預發泡程序之前，被施用於聚合物粒子表面上。已經證實特別適用的黏著促進劑是聚醯胺或聚(甲基)丙烯酸酯。但是，就複合材料之產製，特別是依據外層所用基質材料所需，也可以使用嫻於此技術者已知的低分子量化合物。
特別地，本發明方法之重要的優點在於其可極迅速進行，並因此而有非常低的循環時間。本發明之方法因此可以非常成功地整合於大量製造系統內。
在任何個別情況和其設計中，選用於本發明之整體方法的方法參數取決於所用系統，且亦取決於所用材料。藉由進行些許的初步實驗，嫻於此技術者可輕易地決定這些參數。
較佳地，根據本發明之材料是P(M)I，特別是PMI。這些P(M)I發泡體亦被稱為剛性發泡體，特徵為特定的韌性。該P(M)I發泡體通常以二階段方法製造：a)鑄塑聚合物之製造，和b)該鑄塑聚合物之發泡。根據先前技術，之後經切割或切鋸以得到所欲形狀。或者，在工業中尚未非常廣泛使用的替代方案是根據本發明修飾之模具內發泡。
本發明之方法較佳地使用未預發泡的P(M)I粒子，這些的尺寸由0.5至5.0mm，較佳由1.0至4.0 mm。
在用於本發明之方法之前，可藉兩個不同的方法變體製造該未預發泡的P(M)I粒子。第一個變體中，藉由研磨半完成的P(M)I產物，得到細粒狀的P(M)I粒子。此半完成的P(M)I產物是前述未發泡的聚合物片，以鑄塑聚合物形式得到。
鑄塑聚合物之製造始於包含作為主要構份之(甲基)丙烯酸和(甲基)丙烯腈，其莫耳比較佳是由2：3至3：2，之單體混合物的製造。也可以使用其他共聚單體，例子為丙烯酸或甲基丙烯酸的酯類、苯乙烯、順丁烯二酸和衣康酸和其酐類、及乙烯基吡咯烷酮。但是，這些共聚單體的比例不應超過30重量%。也可以使用小量的交聯單體，例如丙烯酸烯丙酯。但是，其量應較佳地為至多0.05重量%至2.0重量%。
共聚反應混合物另包含起泡劑，其於約15至250℃的溫度，分解或蒸發並因此形成氣相。聚合反應於低於此溫度發生，鑄塑聚合物因此包含潛在的起泡劑。此聚合反應有利地發生於介於兩個玻璃板之間的厚片模具中。
此類型之半完成的PMI產物之製造為嫻於此技術者基本上已知者且可見於例如EP 1 444 293、EP 1 678 244或WO 2011/138060。可特別提及之半完成的PMI產物是Evonik Industries AG以商標名稱ROHACELL®以發泡形式售於市面者。就產製和加工而 言，半完成的丙烯醯亞胺產物(半完成的PI產物)可被視為PMI發泡體的同系物。但是，就毒理學因素，對於丙烯醯亞胺發泡體的喜愛程度遠不及對於其他發泡體材料的喜愛程度。
本發明之方法的第二個變體中，該P(M)I粒子是懸浮聚合物，其可被直接引至方法中。此類型的懸浮聚合物之製造可見於例如DE 18 17 156或德國專利申請案第13155413.1號。
較佳地，預發泡的P(M)I粒子的整體密度是由40至400kg/m3，較佳地由60至300kg/m3，且特別佳地由80至220kg/m3。
預發泡的P(M)I粒子的最大尺寸另較佳地由1.0至25mm，特別佳地由2.0至20mm。
除了所述方法以外，本發明亦提出自該方法得到的所述發泡體，特別是P(M)I發泡體。這些的特徵在於該發泡體包含鋁、銀、銅、鎂、碳纖維、氧化鋁、氮化鋁、碳化矽、氮化硼或這些的混合物。
根據本發明製造的聚合物發泡體，特別是P(M)I發泡體，可經進一步加工以提供發泡體模塑物或發泡體-芯複合材料。該發泡體模塑物或發泡體-芯複合材料特別可用於大量生產，例如用於車身建造或用於汽車工業的內部包覆、軌道載具建構或造船、航空工業、機械工程的內部零件、運動設備製造、傢俱建構或風力發電機組設計。

Claims (16)

  1. 一種用於聚合物粒子之模具內發泡的方法，其特徵在於將聚合物粒子或預發泡的聚合物粒子a)引至模具，b)於發泡溫度T1發泡，c)冷卻，和d)在移除溫度T2移除最終的發泡部件，其中該聚合物粒子包含基質材料、至少一種起泡劑和導熱性填料。
  2. 如申請專利範圍第1項之方法，其中該基質材料係PMI、PI、PP、PU或PVC，較佳為PMI或PI。
  3. 如申請專利範圍第1或2項之方法，其中該導熱性填料至少某些程度地位於該聚合物粒子內。
  4. 如申請專利範圍第1至3項中任一項之方法，其中該導熱性填料至少某些程度地位於該聚合物粒子的表面上。
  5. 如申請專利範圍第1至4項中任一項之方法，其中該導熱性填料係鋁、銀、銅、鎂、碳纖維、氧化鋁、氮化鋁、碳化矽、氮化硼或這些的混合物。
  6. 如申請專利範圍第1至5項中任一項之方法，其中該填料為粉末、球、小板、薄片或長粒的形式。
  7. 如申請專利範圍第1至6項中任一項之方法，其中該起泡劑係醇、烷、烯、酮、醛或這些的混合物，該起泡劑於標準壓力的沸點是35至150℃。
  8. 如申請專利範圍第1至7項中任一項之方法，其中該起泡劑是包含至少一種在發泡條件下經由化學反應釋出揮發性化合物的起泡劑之混合物。
  9. 如申請專利範圍第8項之方法，其中該釋出起泡劑的化合物係共聚至該基質材料中的三級丁醇、異丙醇、或(甲基)丙烯酸異丙酯或(甲基)丙烯酸三級丁酯。
  10. 如申請專利範圍第1至9項中任一項之方法，其中發泡溫度T1是由120至300℃。
  11. 如申請專利範圍第1至9項中任一項之方法，其中未發泡的聚合物粒子藉使用紅外射線預發泡，該紅外射線之至少80%的波長是由1.4至10.0μm，之後材將該預發泡的粒子引至模具。
  12. 如申請專利範圍第11項之方法，其中未經預發泡之聚合物粒子的尺寸是由0.5至5.0mm。
  13. 如申請專利範圍第1至12項中任一項之方法，其中發泡期間至多2分鐘，步驟a)至d)一起進行3至30分鐘。
  14. 如申請專利範圍第1至13項中任一項之方法，其中在步驟a)中，粒子被抽吸和/或吹入模具中，使得模具中粒子的充填程度為50至100%。
  15. 一種P(M)I發泡體，其包含鋁、銀、銅、鎂、碳纖維、氧化鋁、氮化鋁、碳化矽、氮化硼或這些的混合物。
  16. 一種藉由申請專利範圍第1至14項中任一項之方法製造的發泡體之用途，其係用於製造太空船、飛機、船、軌道載具、陸地載具、風車或運動設備。
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