TW201529713A - 具有對聚胺基甲酸酯層改良黏著性之聚碳酸酯組成物 - Google Patents
具有對聚胺基甲酸酯層改良黏著性之聚碳酸酯組成物 Download PDFInfo
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- TW201529713A TW201529713A TW103135768A TW103135768A TW201529713A TW 201529713 A TW201529713 A TW 201529713A TW 103135768 A TW103135768 A TW 103135768A TW 103135768 A TW103135768 A TW 103135768A TW 201529713 A TW201529713 A TW 201529713A
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- Laminated Bodies (AREA)
Abstract
本發明有關於一種組成物,包含A)30至45重量份的至少一種聚合物,選自包括芳香族聚碳酸酯與芳香族聚酯碳酸酯之構成組群,B)32至54重量份的至少一種聚對苯二甲酸伸烷基酯(polyalkylene terephthalate),較佳為聚對苯二甲酸丁二酯,C)16至23重量份的至少一種混合物,包含至少一種含有聚丁二烯的乙烯基(共)聚合物與至少一種不含聚丁二烯的乙烯基(共)聚合物,D)0.1至20.0重量份(以於各情況下成分A至C之總和為基準)的至少一種聚合物添加劑,於此該聚丁二烯含量以成分A至C之重量份總和為基準為8%至18%(以重量計),及於此來自成分C之不含丁二烯的乙烯基(共)聚合物之總含量以成分A至C之重量份總和為基準為3%至12%(以重量計),及於此在該聚碳酸酯組成物中的成分A至C之重量份總和被標定至100,及一種形成自這些組成物與一聚胺基甲酸酯層之複合組件,其在二個層體間的改良黏著性係顯著的,及一種製造該複合組件之方法。
Description
本發明提供對聚胺基甲酸酯系統具有改良黏著性之聚碳酸酯組成物,包含這些聚碳酸酯組成物與聚胺基甲酸酯系統之複合體系統(composite system),還有形成自這些複合體系統之成形體及用於製造該複合體系統之方法。該聚碳酸酯組成物不僅僅對在溫度變化試驗後的聚胺基甲酸酯系統的良好黏著性是顯著的,而且對高的低溫韌性、高的耐熱變形性、高的彈性之模量、還有高的斷裂時伸長率(elongation at break)及低的整體收縮率(overall shrinkage)係為顯著的。
WO 2006/072366 A1敘述一種在具有至少兩個空穴之模塑體(mould)中形成及塗布一基材之方法。該方法包含下述步驟:a)在該模塑體之第一空穴中形成一基材,b)將前述步驟中製得的基材引入該模塑體之第二空穴內及c)以一塗層材料塗布在該第二空穴中的基材,該塗布係在升高壓力下實行。
藉由實施例及優選之方式,述及的有聚胺基甲酸酯塗層材料及PC+ABS基材(聚碳酸酯+丙烯腈-丁二烯-苯乙烯基材)。於這申請案中沒有任何指示(pointers)予以關於該載體材料組成物在該材料複合物(material composite)之黏著性質上的影響。
EP 2089207 A1揭示一種製造一複合組件(composite component)(尤其是包含一注射模塑體(injection moulding)與一聚胺基甲酸酯元件)之方法,包
含下述步驟a)製造一載體組件,b)將該載體組件移動或轉移至一模塑體之開啟的空穴,c)閉合該模塑體至一預定位置,生成一具有第一尺寸之擴大的空穴,d)於該第一尺寸之擴大的空穴中產生一下降的壓力,e)將一灌注材料(flooding material)引入該擴大的空穴內及f)與該灌注材料之引入同時及/或在引入之後進行壓紋(embossing)步驟,同時至少稍微地減小該空穴的尺寸。
為改良該複合體黏著性,在此敘述藉火焰、電漿處理或氣體活化該熱塑性塑膠表面。於這公開案中沒有任何指示予以關於該載體材料組成物在該材料複合物之黏著性質上的影響。
DE 10 2006 033 059 A1揭示一種製造塑膠內部組件之方法。於這方法,於第一步驟中,該載體被形成於第一模塑體中,然後該第一模塑體至少部分被第二模塑體替代及之後於第二步驟中的載體上形成頂層。所用的載體材料為一硬質成分,e.g.PA+ABS摻合物(聚醯胺+丙烯腈-丁二烯-苯乙烯)或PC+ABS摻合物(聚碳酸酯+丙烯腈-丁二烯-苯乙烯),及所用的頂層為軟質成分,較佳為聚胺基甲酸酯發泡體。於這申請案中沒有任何指示予以關於該載體材料之組成物在該如此製得的組件之複合性質上的影響。替代的是,DE 10 206 033 059 A1同時提出藉底料(primer)或藉雷射、電暈或電漿處理製備該表面而改良黏著性。
WO 99/20464揭示彼此直接接合的至少兩種不同聚合物材料之複合體:a)一熱塑性聚合物或一聚合物之熱塑性塑膠混合物,其含有週期表主族1至5或週期表過渡金屬族1至8之至少一種金屬的至少一種極性化合物作為超細分布的無機粉末,與b)以一發泡體、塗層材料或壓實材料之形式存在的聚胺基甲酸酯。對該複合體不需要任何黏著性促進層。就ABS含量與橡膠含量而論於這公開案中沒有任何指示予以關於該載體材料組成物在該材料複合物之黏著性質上的影響。
DE 101 09 226 A1揭示一種聚碳酸酯組成物,包含a)芳香族聚碳酸酯及/或聚酯碳酸酯,b)接枝聚合物及c)苯乙烯與一含有羧基之單體之共聚物,於此所述共聚物具有一平均分子量(mean molecular weight)Mw為>=10 500g/mol,及於此所述共聚物可含有一或多種乙烯基單體。成分C較佳為苯乙烯與順丁烯二酸酐之共聚物。DE 101 09 226 A1另揭示複合組件,包含至少一第一層(1)及一第二層(2),其中層(1)包括至少一種聚碳酸酯組成物(如於a、b及c中所特定的)及層(2)含有至少一種聚胺基甲酸酯。該複合體特性為,在一雙重交替環境試驗(double alternating climate test)之後介於層(1)與層(2)間的發泡體黏著性下降為最多35%。就ABS含量與橡膠含量而論於這公開案中沒有任何指示予以關於該載體材料組成物在該材料複合物之黏著性質上的影響。
本發明之目的係為了提供在溫度變化試驗後對聚胺基甲酸酯系統具有良好黏著性之改良的聚碳酸酯組成物,包含這些聚碳酸酯組成物及聚胺基甲酸酯層之複合體系統,及形成自這些複合體系統之成形體。聚碳酸酯組成物在溫度變化試驗後對該聚胺基甲酸酯系統之良好黏著性、及對高的低溫韌性、高的耐熱變形性、高的彈性之模量、還有高的斷裂時伸長率及低的整體收縮率係為顯著的。
此外,係為了提供一種用於製造這些複合組件之方法。
該聚胺基甲酸酯層可用來,例如,改良該複合組件之表面性質,例如耐刮擦性、自行復原性(self-healing)、風化穩定性、觸覺(tactile)性質、光學性質、隔音及隔熱。
達成本發明之目的係藉聚碳酸酯組成物,其包含A)30至45重量份,較佳地32至45重量份,更佳地35至45重量份,的至少一種聚合物,選自包括芳香族聚碳酸酯與芳香族聚酯碳酸酯之構成組群,B)32至54重量份,較佳地32至50重量份,更佳地32至45重量份,的至
少一種聚對苯二甲酸伸烷基酯,較佳為聚對苯二甲酸丁二酯,C)16至23重量份,較佳地17至22重量份,更佳地18至21重量份,的至少一種混合物,包含至少一種聚丁二烯系接枝聚合物與至少一種不含丁二烯的乙烯基(共)聚合物,D)0.1至20.0重量份,較佳地0.2至15.0重量份,更佳地0.3至10.0重量份(以於各情況下成分A至C之總和為基準),的至少一種聚合物添加劑,於此該聚丁二烯含量以成分A至C之重量份總和為基準為8%至18%(以重量計),較佳地9%至17%(以重量計),更佳地10%至16%(以重量計),及於此來自成分C之不含丁二烯的乙烯基(共)聚合物之總含量以成分A至C之重量份總和為基準為3%至12%(以重量計),較佳地4%至11%(以重量計),更佳地5%至10%(以重量計),及於此在該聚碳酸酯組成物中的成分A至C之重量份總和被標定至100。
圖1顯示根據本發明方法製造複合組件之實施例說明。
當所提及的適宜範圍可與彼此隨意組合時,適宜予以與各個第一、中間及最後範圍彼此組合。
於一另外較佳具體實施,該聚碳酸酯組成物不含填充劑與強化劑,例如滑石、玻璃纖維或碳纖維(選擇地包括研磨的纖維)、(中空)玻璃或陶瓷珠、雲母、高嶺土、CaCO3及玻璃碎片。
於一另外較佳具體實施,該聚碳酸酯組成物包含A)30至45重量份的至少一種聚合物,選自包括芳香族聚碳酸酯與芳香族聚酯碳酸酯之構成組群,B)32至54重量份的至少一種聚對苯二甲酸丁二酯,C)16至23重量份的至少一種混合物,包含至少一種聚丁二烯系接枝聚
合物與至少一種不含丁二烯的乙烯基(共)聚合物,D)0.1至20.0重量份(以於各情況下成分A至C之總和為基準)的至少一種聚合物添加劑,於此該聚丁二烯含量以成分A至C之重量份總和為基準為8%至18%(以重量計),及於此來自成分C之不含丁二烯的乙烯基(共)聚合物之總含量以成分A至C之重量份總和為基準為3%至12%(以重量計),及於此成分C之接枝聚合物,以該接枝聚合物為基準,包含20%至55%(以重量計)的至少一種乙烯基單體與80%至45%(以重量計)的一或多種聚丁二烯系接枝基質(graft bases),及於此該接枝聚合物係藉乳化聚合反應製備的,及於此該聚丁二烯系接枝聚合物之接枝基質具有一中值粒子大小(d50)為0.2至1.0μm,其藉超離心方法測得,及於此至少兩種穩定劑被用於成分D中,於此該第二穩定劑包含一Brnsted-酸系化合物,及於此在該聚碳酸酯組成物中的成分A至C之重量份總和被標定至100。
於一另外較佳具體實施,該聚碳酸酯組成物不含滯焰劑及不含滯焰劑協同劑,諸如抗滴劑。於一另外較佳具體實施,該聚碳酸酯組成物只由成分A、B、C及D構成。
此外且適宜者,本發明之目的係藉包含下述之複合組件達成的,a)一載體,由一如上述特定的聚碳酸酯組成物所構成b)至少一種聚胺基甲酸酯層。
所述聚胺基甲酸酯層可,例如,為一PU塗層材料、一PU發泡體或者是一具有聚胺基甲酸酯層厚度為(例如)1μm至多20cm之壓實PU皮。
於一較佳具體實施,該聚胺基甲酸酯層為一具有層厚度為1至1000μm之塗層材料,另較佳地10至500μm及更佳地50至300μm。
於一另外較佳具體實施,該聚胺基甲酸酯層為一具有層厚度為1mm至20cm之發泡體,另較佳地1mm至10cm及更佳地1mm至1cm。
於一另外較佳具體實施,該聚胺基甲酸酯層為一具有層厚度為0.5mm至10.0mm之壓實皮,較佳地0.5mm至5.0mm及更佳地1.0mm至4.0mm。
該複合組件原則上可以任何已知方式被製造。
較佳地,該聚胺基甲酸酯層係藉包含下述之反應性聚胺基甲酸酯原料混合物之完全聚合反應製造的- 至少一種聚異氰酸酯成分,- 至少一種多官能性H-活性化合物,及- 選擇地至少一種聚胺基甲酸酯添加劑及/或加工助劑,係與事先已成形自該熱塑性塑膠組成物及已被固化的載體直接接觸。
該載體組件可預製(例如)自該熱塑性PC+ABS組成物及該反應性聚胺基甲酸酯原料混合物可被施用至其且完全反應。根據該聚胺基甲酸酯反應成分之反應性,它們可先已被預混合或在施用期間可以已知方式被混合。該施用可藉包括噴塗(spraying)、刀-塗布或軋光(calendaring)之方法實行。
若欲製得發泡的複合體,可以本身已知方式將該反應混合物引入一含有預先形成的及固化的支撐組件(support component)之模塑體內。選擇地,該模塑體還可含有一另外的裝飾層(decorative layer)(通常稱為"皮"),其由(例如)聚氯乙烯(PVC)、熱塑性聚烯烴類(TPO)、熱塑性聚胺基甲酸酯(TPU)或可噴塗的聚胺基甲酸酯皮所構成。於該模塑體中,該可發泡的反應混合物發泡體係與該載體組件及任意的裝飾層接觸,及形成該複合組件。該模
塑體內(in-mould)發泡可依諸如該複合組件在它的表面具有一胞孔結構(cell structure)之方式實施。或者是,可依諸如該複合組件具有一壓實皮及一蜂窩芯(cellular core)(積合發泡體(integral foams))之方式進行。利用高壓或低壓機器可將該聚胺基甲酸酯成分引入該模塑體內。
聚胺基甲酸酯發泡體還可被製成塊狀發泡體(slabstock foam)。
聚胺基甲酸酯複合體還可以夾層(sandwich)模式被製造。該方法可被組態成或為庫式方法(depot method)或為殼建式方法(shell-building method)。該庫式方法及該殼建式方法本身均是已知的。於該庫式方法(填充模式)中,兩個半殼(例如製自聚合物之外層)被預製及被插入一模塑體內,及介於殼體之間的空穴藉以PUR發泡體發泡填充。於殼建式模式中,PUR發泡體核芯被置於一模塑體中及之後包裹有適合的殼材料,例如提及的熱塑性塑膠之一者。於夾層複合體之製造中,適宜為予以殼建式模式。
於本發明之一較佳具體實施,該複合組件係藉一方法製得,其中(i)於第一方法步驟中,將該熱塑性塑膠組成物之熔體注入一第一模塑體空穴內及之後冷卻,(ii)於第二方法步驟中,將該熱塑性塑膠成分轉移至一較大空穴內及藉此製得一界定的間隙(defined gap),(iii)於第三方法步驟中,於該熱塑性塑膠成分與該擴大的空穴之模塑體表面之間所產生的間隙注入有一包含下述之反應性聚胺基甲酸酯原料混合物- 至少一種聚異氰酸酯成分,- 至少一種多官能性H-活性化合物,及- 選擇地至少一種聚胺基甲酸酯添加劑及/或加工助劑,該聚胺基甲酸酯原料混合物係以與該熱塑性塑膠載體的表面直接接觸之方式完全聚合,以得到一壓實聚胺基甲酸酯層或得到一聚胺基甲酸酯發泡體層,及(iv)於第四方法步驟中,該複合組件自該模塑體空穴中被脫模。
於本發明之一另外較佳具體實施,方法步驟(i)至(iv)在該複合組件製造中彼此緊接著依序跟隨。
若需要的話,該較大空穴在方法步驟(iii)之前利用一分離劑處理。
該方法步驟之緊接著次序係避免在該方法期間該工件(workpiece)冷卻降到室溫。這達到製造次數上的減少及該整體方法之較高能量效益。
隨著該聚胺基甲酸酯系統之變化,方法步驟(ii)及(iii)可被重複至少一次,於其情況下一或多種聚胺基甲酸酯層被施用至該載體之一或兩面上,以使產生一由熱塑性塑膠載體與至少兩種相同或不同的PU組件所構成的複合組件,該PU組件可選擇地還具有多於二-層結構。
在步驟(ii)及(iv)中的工件脫模之前,該工件被降溫直到它為尺寸上穩定的。
為於方法步驟(ii)中製造該間隙,可以開啟該注射模塑體及隨後將一半的注射模塑體空穴換成具較高空穴尺寸之新的一半注射模塑體空穴,或將該組件自該第一模塑體空穴移動至一第二空穴(就它的空穴尺寸而論係較大的)或至一第二模塑體,或開啟該欲產生一間隙之第一空穴。
於方法步驟(ii)中該基材之移動作用可藉已知方法實行,如以(例如)多色(multicolour)注射模塑施用。典型方法為首先利用一轉盤(turntable)、一轉板(turning plate)、一滑動空穴或一指標板(index plate)移動,或其中該基材保留在一核芯上之可相比擬的方法。若該用於移動之基材保留在該核芯上時,這具有即使在移動之後準確界定該位置之優點。其次,先前技術揭示用於移動一基材之方法,其中該基材係例如借助一操控系統自一空穴去除,及被置入另一空穴內。隨著該基材去除之移動在該塗布操作中提供更高的組態自由度,例如產生一摺邊(edge fold)或遮蔽區域(masked region)。
於一較佳具體實施,於該第一方法步驟中,使用一熱塑性聚合物組成物,在依ISO 180-1 A之缺口衝擊性試驗(notched impact test)中,其在室溫下及更佳地還在-20℃下,具有高韌性,特徵在於耐缺口衝擊性值為高於30kJ/m2。
用於本發明複合組件之製造的反應性聚胺基甲酸酯原料混合物較佳具有一指數為>80至<125,另較佳地>90至<120,及更佳地100至110。
該指數被定義為,實際上使用的異氰酸酯之用量對在與該H-活性多官能性成分之完全反應情況下計算的化學計量之百分比例,i.e.指數=(使用的異氰酸酯用量/異氰酸酯之計算的化學計量)* 100。
於一另選具體實施,它還可以使用一熱塑性聚胺基甲酸酯,而不是該反應性聚胺基甲酸酯原料混合物。
於一另外較佳具體實施,與該熱塑性聚合物組成物接觸的注射模塑體之表面於方法步驟(iii)中被加熱至50至100℃範圍之溫度,較佳地55至95℃,及更佳地60至90℃。
於一另外較佳具體實施,與該反應性聚胺基甲酸酯混合物接觸的注射模塑體之表面於方法步驟(iii)中被加熱至50至160℃範圍之溫度,較佳地50至120℃,另較佳地60至110℃,及更佳地60至90℃。
於一另外較佳具體實施,與該熱塑性聚合物組成物接觸的注射模塑體之表面於方法步驟(iii)中被加熱至50至100℃範圍之溫度,較佳地55至95℃,及更佳地60至90℃,及與該反應性聚胺基甲酸酯混合物接觸的注射模塑體之表面被加熱至50至160℃範圍之溫度,較佳地50至120℃,另較佳地60至110℃,及更佳地60至90℃。
若涵蓋一具裝飾層之發泡的聚胺基甲酸酯系統時,於一另選具體實
施,與該熱塑性聚合物組成物接觸或與該裝飾皮接觸的發泡模塑體之表面可被加熱至20至80℃範圍之溫度,較佳地30至60℃。
本發明複合組件特別適合作為鐵路車輛、飛機或汽車之內部或外部組件,及適合作為電氣/電子組件。
於本發明複合組件中,介於該由聚碳酸酯組成物所構成的載體與該聚胺基甲酸酯塗層之間的複合體黏著性,於一較佳具體實施,係為至少1N/mm,依DIN EN 1464以一100mm/min運行速度(traversing speed),於一浮動輥(floating roller)試驗中,在取自該組件之具有20mm寬度的條狀樣品上測得。
用於根據本發明方法中的聚合物組成物包含:
成分A
依照本發明適合的成分A之芳香族聚碳酸酯類及/或芳香族聚酯碳酸酯類為文獻上已知的或可藉文獻上已知的方法製備(用於芳香族聚碳酸酯類之製備見,例如,Schnell,"Chemistry and Physics of Polycarbonates",Interscience Publishers,1964,還有DE-B 1 495 626、DE-A 2 232 877、DE-A 2 703 376、DE-A 2 714 544、DE-A 3 000 610、DE-A 3 832 396;用於芳香族聚酯碳酸酯類之製備,例如DE-A 3 077 934)。
製備芳香族聚碳酸酯類及聚酯碳酸酯類係,例如,藉使二酚類與碳酸系鹵化物(carbonic halides)(較佳地光氣)、及/或與芳香族二羰基二鹵化物(較佳地苯二羰基二鹵化物)之反應,藉界面方法,選擇地使用鏈終止劑,例如單酚類,及選擇地使用三官能性或多於三官能性支化劑,例如三酚類或四酚類。經由熔體聚合反應方法透過二酚類與(例如)碳酸二苯酯的反應,其製備同樣可行。
用於該芳香族聚碳酸酯類及/或芳香族聚酯碳酸酯類之製備的二酚類較佳為彼等式(I)
式中A 為一單鍵、C1至C5-伸烷基、C2至C5-亞烷基、C5至C6-環亞烷基、-O-、-SO-、-CO-、-S-、-SO2-、C6至C12-伸芳基,可稠合另外的選擇性含有雜原子之芳香族環至其上,或一式(II)或(III)之自由基
B 於各情況下為C1至C12-烷基(較佳地甲基)、鹵素(較佳地氯及/或溴),,x 於各情況下獨立地為0、1或0,p 為1或0,及R5及R6可獨立地被選用於各X1,及各獨立地為氫或C1至C6-烷基,較佳地氫、甲基或乙基,X1 為碳及m 為4至7之整數,較佳地4或5,其條件為在至少一個X1原子上的R5及R6同時為烷基。
較佳的二酚類為氫醌(hydroquinone)、間苯二酚(resorcinol)、二羥基二酚
類、雙(羥基苯基)-C1-C5-烷類、雙(羥基苯基)-C5-C6-環烷類、雙(羥基苯基)醚類、雙(羥基苯基)亞碸類(sulphoxides)、雙(羥基苯基)酮類、雙(羥基苯基)碸類(sulphones)及α,α-雙(羥基苯基)二異丙基苯類,及其環-溴化的及/或環-氯化的衍生物。
特佳的二酚類為4,4’-二羥基二苯基、雙酚A、2,4-雙(4-羥基苯基)-2-甲基丁烷、1,1-雙(4-羥基苯基)環己烷、1,1-雙(4-羥基苯基)-3,3,5-三甲基環己烷、4,4’-二羥基二苯基硫化物、4,4’-二羥基二苯基碸及其二-與四溴化的或-氯化的衍生物,例如2,2-雙(3-氯-4-羥基苯基)丙烷、2,2-雙(3,5-二氯-4-羥基苯基)丙烷或2,2-雙(3,5-二溴-4-羥基苯基)丙烷。尤佳的是2,2-雙(4-羥基苯基)丙烷(雙酚A)。
可以單獨地或以任何所希望的混合物之形式使用二酚類。該二酚類為文獻上已知的或可藉文獻上已知方法獲得。
適用於該熱塑性芳香族聚碳酸酯類製備之鏈終止劑實例包括酚、p-氯酚、p-tert-丁基酚或2,4,6-三溴酚,而還有長鏈烷基酚類諸如4-[2-(2,4,4-三甲基戊基)]酚、4-(1,3-四甲基丁基)酚(根據DE-A 2 842 005),或於該烷基取代基中具有總數8至20個碳原子之單烷基酚類或二烷基酚類,諸如3,5-二-tert-丁基酚、p-異辛基酚、p-tert-辛基酚、p-十二烷基酚及2-(3,5-二甲基庚基)酚及4-(3,5-二甲基庚基)酚。欲被使用的鏈終止劑之用量一般介於0.5mol%至10mol%,於各情況下以所用的二酚類之莫耳和為基準。
該熱塑性芳香族聚碳酸酯類可為以已知方式分支的,較佳地透過合併0.05至2.0mol%的三官能性或多於三官能性化合物,例如彼等具有三個或以上酚系基團,以所用的二酚類之總和為基準。
均聚碳酸酯類及共聚碳酸酯類均適合。對本發明成分A之共聚碳酸酯類之製備,還可以使用1%至25%(以重量計),較佳地2.5%至25%(以重量計)的具有羥基芳氧基端基之聚二有機矽氧烷類,以所用的二酚類之總用量為
基準。這些係已知的(US 3 419 634)及可藉由文獻上已知的方法製備。含有聚二有機矽氧烷之共聚碳酸酯類的製備敘述於DE-A 3 334 782。
較佳的聚碳酸酯類(以及該雙酚A均聚碳酸酯類)為雙酚A與至多15mol%(以二酚類之莫耳和為基準)的其它二酚類(具體為較佳的或特佳的、尤其是2,2-雙(3,5-二溴-4-羥基苯基)丙烷)之共聚碳酸酯類。
用於芳香族聚酯碳酸酯類製備之芳香族二羰基二鹵化物較佳為間苯二甲酸、對苯二甲酸、二苯基醚4,4’-二羧酸及萘-2,6-二羧酸之二酸二氯化物。
特別適宜為予以該以介於1:20至20:1比例的間苯二甲酸與對苯二甲酸之二酸二氯化物之混合物。
於聚酯碳酸酯類之製備中,碳酸系鹵化物(較佳地光氣)還用作為雙官能性酸衍生物。
可用於該芳香族聚酯碳酸酯類之製備的鏈終止劑包括(除了已述及的單酚類外)其氯碳酸系酯類及該芳香族單羧酸之酸氯化物,其可選擇性被C1至C22-烷基或被鹵素原子所取代,及脂族C2至C22-單羰基氯化物。
於各情況下該鏈終止劑之用量為0.1至10mol%,以於酚系鏈終止劑情況下的二酚莫耳數及以於單羰基氯化物鏈終止劑情況下的二羰基二氯化物之莫耳數為基準。
該芳香族聚酯碳酸酯類還可含有合併的芳香族羥基羧酸類。
該芳香族聚酯碳酸酯類可以已知方式或為線性或為分支的(見DE-A 2 940 024及DE-A 3 007 934)。
所用的支化劑可,例如,為三-或多官能性羰基氯化物,諸如三甲磺醯
基三氯化物(trimesyl trichloride)、三聚氰胺三氯化物(cyanuric trichloride)、3,3’,4,4’-二苯甲酮四羰基四氯化物、1,4,5,8-萘四羰基四氯化物或苯均四甲酸四氯化物,以0.01至1.0mol%之用量(以所用的二羰基二氯化物為基準),或三-或多官能性酚類,諸如間苯三酚(phloroglucinol)、4,6-二甲基-2,4,6-三(4-羥基苯基)庚-2-烯、4,6-二甲基-2,4-6-三(4-羥基苯基)庚烷、1,3,5-三(4-羥基苯基)苯、1,1,1-三(4-羥基苯基)乙烷、三(4-羥基苯基)苯基甲烷、2,2-雙[4,4-雙(4-羥基苯基)環己基]丙烷、2,4-雙(4-羥基苯基異丙基)酚、四(4-羥基苯基)甲烷、2,6-雙(2-羥基-5-甲基苄基)-4-甲基酚、2-(4-羥基苯基)-2-(2,4-二羥基苯基)丙烷、四(4-[4-羥基苯基異丙基]苯氧基)甲烷、1,4-雙[4,4’-二羥基三苯基)甲基]苯,以0.01至1.0mol%之用量,以所用的二酚類為基準。酚系支化劑最初可與該二酚類一起進料;酸氯化物支化劑可與該酸二氯化物一起被引入。
於該熱塑性芳香族聚酯碳酸酯類中的碳酸酯構造單元之比例可如所希望的變化。較佳地,該碳酸酯基團之比例為至多100mol%,尤其是至多80mol%,更佳地至多50mol%,以酯基團與碳酸酯基團之總和為基準。該芳香族聚酯碳酸酯類之酯部分及碳酸酯部分在該聚縮合物中均可以嵌段或以無規分布之形式存在。
芳香族聚碳酸酯類及聚酯碳酸酯類之相對溶液黏度(ηrel)較佳於1.18至1.4之範圍,更佳於1.20至1.32之範圍(在25℃下,於0.5g的聚碳酸酯或聚酯碳酸酯於100ml的二氯甲烷之溶液中測量)。該芳香族聚碳酸酯類及聚酯碳酸酯類之重量平均分子量Mw較佳於15 000至35 000之範圍,另較佳於20 000至33 000之範圍,更佳地23 000至30 000,係藉GPC(凝膠滲透層析法,於二氯甲烷中,以聚碳酸酯作為標準品)測定。
成分B
根據本發明,成分B包含聚對苯二甲酸伸烷基酯類。於一較佳具體實施,這些為芳香族二羧酸之反應產物或其反應性衍生物,諸如二甲基酯類或酸酐類,及脂族、環脂族或芳脂族二醇類及這些反應產物之混合物。
特佳的聚對苯二甲酸伸烷基酯類含有至少80重量%、較佳地至少90重量
%(以該二羧酸成分為基準)的對苯二甲酸自由基與至少80重量%、較佳地至少90重量%(以該二醇成分為基準)的乙二醇及/或丁烷-1,4-二醇自由基。
該較佳的聚對苯二甲酸伸烷基酯類可(以及對苯二甲酸自由基)含有至多20mol%(較佳地至多10mol%)的具有8至14個碳原子的其它芳香族或環脂族二羧酸之自由基或具有4至12個碳原子的脂族二羧酸之自由基,例如鄰苯二甲酸、間苯二甲酸、萘-2,6-二羧酸、4,4'-二苯基二羧酸、丁二酸、己二酸、癸二酸、壬二酸、環己烷二乙酸之自由基。
該較佳的聚對苯二甲酸伸烷基酯類可(以及乙二醇及丁烷-1,4-二醇自由基)含有至多20mol%(較佳地至多10mol%)的具有3至12個碳原子的其它脂族二醇類或具有6至21個碳原子的環脂族二醇類,例如丙烷-1,3-二醇、2-乙基丙烷-1,3-二醇、新戊二醇、戊烷-1,5-二醇、己烷-1,6-二醇、環己烷-1,4-二甲醇、3-乙基戊烷-2,4-二醇、2-甲基戊烷-2,4-二醇、2,2,4-三甲基戊烷-1,3-二醇、2-乙基己烷-1,3-二醇、2,2-二乙基丙烷-1,3-二醇、己烷-2,5-二醇、1,4-二(β-羥基乙氧基)-苯、2,2-雙(4-羥基環己基)丙烷、2,4-二羥基-1,1,3,3-四甲基環丁烷、2,2-雙(4-β-羥基乙氧基苯基)丙烷及2,2-雙(4-羥基丙氧基苯基)丙烷之自由基(DE-A 2 407 674、2 407 776、2 715 932)。
該聚對苯二甲酸伸烷基酯類可藉合併入相當少量的3-或4-元醇類或3-或4-元羧酸類而被分支,例如根據DE-A 1 900 270及US-A 3 692 744。較佳的分支劑實例為苯三酸(trimesic acid)、偏苯三酸(trimellitic acid)、三羥甲基乙烷與-丙烷及季戊四醇。
特別適宜予以僅僅係已製備自對苯二甲酸及其反應性衍生物(e.g.其二烷基酯類)與乙二醇及/或丁烷-1,4-二醇之聚對苯二甲酸伸烷基酯類,及這些聚對苯二甲酸伸烷基酯類之混合物。
聚對苯二甲酸伸烷基酯類之混合物含有1%至50%(以重量計)、較佳地1%至30%(以重量計)的聚對苯二甲酸乙二酯與50%至99%(以重量計)、較佳地70%至99%(以重量計)的聚對苯二甲酸丁二酯。
該適宜使用的聚對苯二甲酸伸烷基酯類較佳具有固有黏度(intrinsic viscosity)為0.4至1.5dl/g,較佳地0.5至1.2dl/g,於Ubbelohde黏度計中,依DIN 53728-3在25℃下於1重量%濃度二氯乙酸中測得。所測定的固有黏度系計算自所測得的比黏度(specific viscosity)x 0.0006907+0.063096。
特別適宜予以使用聚對苯二甲酸丁二酯作為成分B。
特佳的聚對苯二甲酸丁二酯類具有熔體流動速率(melt flow rate)為9g/10min至60g/10min,依DIN EN ISO 1133在250℃及2.16kg荷重下測得。
該聚對苯二甲酸伸烷基酯類可藉已知方法被製備(見,例如,Kunststoff-Handbuch[Plastics Handbook],volume VIII,p.695 ff.,Carl-Hanser-Verlag,Munich 1973)。
成分C
成分C包含聚丁二烯系接枝聚合物或丁二烯系接枝聚合物與不含丁二烯的乙烯基(共)聚合物之混合物,成分C之丁二烯含量為至少40重量份。
用於成分C之聚丁二烯系接枝聚合物包含
C.1 5%至60%,較佳地15%至58%及尤其是20%至55%(以重量計)的至少一種乙烯基單體,以該接枝聚合物為基準,在
C.2 95%至40%,較佳地85%至42%及尤其是80%至45%(以重量計)的一或多種聚丁二烯系接枝基質上,以該接枝聚合物為基準。
該接枝基質C.2一般具有一中值粒子大小(d50)為0.05至10.00μm,較佳地0.1至5.0μm,更佳地0.2至1.0μm,及最佳地0.2至0.5μm。
該平均粒子大小(mean particle size)d50為50重量%的粒子落在超過或低於其之直徑。它可藉由超離心測量之方式測得(W.Scholtan,H.Lange,Kolloid,Z.and Z.Polymere 250(1972),782-1796)。
單體C.1較佳為下述之混合物
C.1.1 50至99(較佳地65至85,及尤其是75至80)重量份的乙烯基芳香族化合物及/或環-取代的乙烯基芳香族化合物(諸如苯乙烯、α-甲基苯乙烯、p-甲基苯乙烯、p-氯苯乙烯)及/或甲基丙烯酸(C1-C8)-烷基酯類諸如甲基丙烯
酸甲基酯、甲基丙烯酸乙基酯),以C.1為基準,及C.1.2 1至50(較佳地15至35,及尤其是20至25)重量份的乙烯基氰化物(不飽和腈類諸如丙烯腈及甲基丙烯腈)及/或(甲基)丙烯酸(C1-C8)-烷基酯諸如甲基丙烯酸甲基酯、丙烯酸n-丁基酯、丙烯酸t-丁基酯,及/或不飽和羧酸之衍生物(諸如酸酐類及醯亞胺類),例如順丁烯二酸酐及N-苯基馬來醯亞胺,以C.1為基準。
較佳的單體C.1.1為選自該單體苯乙烯、α-甲基苯乙烯及甲基丙烯酸甲基酯之至少一者;較佳的單體C.1.2為選自該單體丙烯腈、順丁烯二酸酐及甲基丙烯酸甲基酯之至少一者。特佳的單體為C.1.1苯乙烯及C.1.2丙烯腈。
適用於成分C中的接枝聚合物之接枝基質C.2為純的聚丁二烯橡膠或聚丁二烯橡膠之混合物或聚丁二烯橡膠之共聚物或其與另外的可共聚的單體(例如根據C.1.1及C.1.2)之混合物,其條件是成分C.2之玻璃轉移溫度為<10℃以下,較佳地<0℃以下,更佳地<-20℃以下。
該玻璃轉移溫度為,根據標準DIN EN 61006,藉由差分熱分析(DSC)之方式,在加熱速率10K/min下測定,以Tg定義為中點溫度(切線方法)。
特佳的接枝基質C.2為純的聚丁二烯橡膠。
於成分C中特佳的接枝聚合物為,例如,ABS或MBS聚合物如敘述(例如)於DE-A 2 035 390(=US A 3 644 574)或於DE-A 2 248 242(=GB-A 1 409 275)或於Ullmanns,Enzyklopädie der Technischen Chemie[Encyclopaedia of Industrial Chemistry],vol.19(1980),p.280 ff。
於成分C中的接枝共聚物係藉自由基聚合反應製備,例如藉乳化或懸浮聚合反應,尤其是藉乳化聚合反應。
在於成分C中的接枝聚合物係已以乳化聚合方法製備之情況下,接枝基
質C.2之含量較佳為20%至95%(以重量計),更佳地40%至85%(以重量計),尤其是50%至75%(以重量計),以於各情況下該接枝聚合物為基準。
該接枝基質C.2之凝膠含量為至少30重量%,較佳地至少40重量%,尤其是至少60重量%,以於各情況下C.2為基準及測量為於甲苯中之不可溶成分。
因為該接枝反應(如熟知的)不需要將該接枝單體完全地接枝至該接枝基質上,根據本發明,於成分C中的接枝聚合物還了解的是意指彼等在接枝基質C.2存在下藉接枝單體C.1之(共)聚合反應得到的產物及還有在處理中得到的產物。這些產物因而還可含有不會化學上鍵結至該聚丁二烯之接枝單體C.1.的自由基(共)聚合物。
該接枝基質C.2或於成分C中的接枝聚合物之凝膠含量係在25℃下於適合溶劑中測定為於不可溶於這些溶劑的成分(M.Hoffmann,H.Krömer,R.Kuhn,Polymeranalytik I und II[Polymer Analysis I and II],Georg Thieme-Verlag,Stuttgart 1977)。
於成分C中不含丁二烯的乙烯基(共)聚合物較佳為至少一種單體之不含丁二烯的均-及/或共聚物C.1,該單體係選自乙烯基芳香族化合物、乙烯基氰化物(不飽和腈類)、(甲基)丙烯酸(C1至C8)-烷基酯類、不飽和羧酸及不飽和羧酸之衍生物(諸如酸酐類及醯亞胺類)之群組。
這些(共)聚合物C.1為樹脂狀、熱塑性且不含丁二烯。更佳地,該共聚物為形成自C.1.1苯乙烯及C.1.2丙烯腈。
這類型的(共)聚合物C.1為已知的及可藉自由基聚合反應製備,尤其是藉乳化、懸浮、溶液或總體聚合反應。該(共)聚合物較佳具有平均分子量Mw(重量-平均,藉GPC測定)介於15 000g/mol至250 000g/mol,較佳於80 000至150 000g/mol之範圍。
成分D
該組成物可包含常用的聚合物添加劑作為成分D。對成分D之可行的常用聚合物添加劑包括添加劑,例如,內部與外部潤滑劑及脫模劑(例如四硬脂酸酯季戊四醇酯、褐煤蠟(montan wax)或聚乙烯蠟)、導電性添加劑(例如導電性黑料或碳奈米管)、穩定劑(例如UV/光穩定劑,熱穩定劑)、成核劑(nucleating agent)(例如苯基膦酸鈉鹽(sodium phenylphosphinate)、氧化鋁、二氧化矽、芳香族羧酸的鹽類)、轉酯化抑制劑(transesterification inhibitors)、抗氧化劑、水解穩定劑)、耐刮擦性-改良添加劑(例如矽酮油或硬質填充劑諸如(中空)陶瓷珠)、IR吸收劑、光學增亮劑、螢光添加劑,還有染料及顏料(例如二氧化鈦、群青(ultramarine blue)、氧化鐵、碳黑、酞青素(phthalocyanine)、喹吖酮(quinacridone)、苝(perylene)、苯胺黑(nigrosin)及蒽醌(anthraquinone)),或者是複數種所述及的添加劑之混合物。
於一較佳具體實施,該組成物包含至少一種添加劑作為成分D,選自包含潤滑劑及脫模劑、成核劑、穩定劑、抗靜電劑、染料、顏料及填充劑與強化劑之組群。
於一另外較佳具體實施,該組成物不包含任何滯焰劑或任何滯焰協同劑(諸如抗滴劑)作為成分D。
更佳地,本發明組成物包含至少一種脫模劑(較佳地四硬脂酸酯季戊四醇酯),較佳地0.1至1.0重量份,以成分A與B之總和為基準,及至少一種穩定劑(較佳為一酚系抗氧化劑),更佳地0.01至1.0重量份的2,6-二-tert-丁基-4-(十八烷氧基羰基乙基)酚,以成分A與B之總和為基準,及/或一有機磷系酯。
另外適宜予以至少兩種穩定劑之穩定劑組合,該第二穩定劑包含一Brnsted-酸系化合物。較佳地,該第二穩定劑為亞磷酸(phosphorous acid)或酸性磷酸酯類,例如單磷酸鈣(calcium monophosphate)。
該添加劑可以單獨或以混合物之形式,或以母料(masterbatches)之形式使用。
聚胺基甲酸酯層
所用的聚胺基甲酸酯層較佳為一聚胺基甲酸酯發泡體或一壓實聚胺基甲酸酯層。
依照本發明使用的聚胺基甲酸酯類係藉使聚異氰酸酯類與H-活性多官能性化合物(較佳地多醇類)之反應而獲得的。
於本發明內文中,該術語"聚胺基甲酸酯"還了解的是意指聚胺基甲酸酯脲類,其中所用的H-活性多官能性化合物為彼等具有N-H官能度之化合物,選擇地為與多醇類之摻合物。
適合的聚異氰酸酯類為本身是此項技術領域熟悉者已知的芳香族、芳脂族、脂族或環脂族聚異氰酸酯類及具有較佳地≧2之NCO官能度,其還可具有亞胺氧雜二嗪二酮、異氰脲酸酯、脲二酮、胺基甲酸酯、脲甲酸酯、縮二脲、脲、氧雜二嗪三酮,氧雜唑烷酮(oxazolidinone)、醯基脲及/或碳二醯亞胺結構。這些可單獨或以與彼此之任何所希望的混合物之形式使用。
前述聚異氰酸酯類係以本身是此項技術領域熟悉者已知的二-或三異氰酸酯類為基底及具有脂族性、環脂族性、芳脂族性及/或芳香族性鍵結的異氰酸酯基團,這些是否係已使用光氣或藉不含光氣之方法製備並不重要。此類二-或三異氰酸酯類之實例為1,4-二異氰酸酯基丁烷、1,5-二異氰酸酯基戊烷、1,6-二異氰酸酯基己烷(HDI)、2-甲基-1,5-二異氰酸酯基戊烷、1,5-二異氰酸酯基-2,2-二甲基戊烷、2,2,4-或2,4,4-三甲基-1,6-二異氰酸酯基己烷、1,10-二異氰酸酯基癸烷、1,3-及1,4-二異氰酸酯基環己烷、1,3-及1,4-雙(異氰酸酯基甲基)環己烷、1-異氰酸酯基-3,3,5-三甲基-5-異氰酸酯基甲基環己烷(異佛爾酮二異氰酸酯,IPDI)、4,4’-二異氰酸酯基二環己基甲烷(Desmodur®
W,Bayer AG, Leverkusen,DE)、4-異氰酸酯基甲基-1,8-辛烷二異氰酸酯(三異氰酸酯基壬烷,TIN)、ω,ω’-二異氰酸酯基-1,3-二甲基環己烷(H6XDI)、1-異氰酸酯基-1-甲基-3-異氰酸酯基甲基-環己烷、1-異氰酸酯基-1-甲基-4-異氰酸酯基甲基環己烷、雙(異氰酸酯基甲基)-降冰片烯、萘1,5-二異氰酸酯、1,3-及1,4-雙(2-異氰酸酯基丙-2-基)苯(TMXDI)、2,4-及2,6-二異氰酸酯基甲苯(TDI),尤其是該2,4及該2,6異構物,及該二種異構物之技術級混合物,2,4’-及4,4’-二異氰酸酯基二苯基甲烷(MDI),聚合性MDI(pMDI),1,5-二異氰酸酯基萘,1,3-雙(異氰酸酯基甲基)苯(XDI)及所述及的化合物之任何所希望的混合物。
該聚異氰酸酯類較佳具有一平均NCO官能度為2.0至5.0,較佳為2.2至4.5,更佳為2.2至2.7,及一異氰酸酯基的含量為5.0%至37.0%(以重量計),較佳為14.0%至34.0%(以重量計)。
於一較佳具體實施,使用上述特定類型的聚異氰酸酯類或聚異氰酸酯混合物,其具有專有脂族性及/或環脂族性鍵結的異氰酸酯基團。
最佳地,上述特定類型的聚異氰酸酯類為以六亞甲基二異氰酸酯、異佛爾酮二異氰酸酯、該異構性雙(4,4’-異氰酸酯基環己基)甲烷類及其混合物為基底。
在相當高分子量的改質的聚異氰酸酯類之中,由聚胺基甲酸酯化學已知的具有終端的異氰酸酯基團及分子量範圍為400至15 000(較佳地600至12 000)之預聚物特別受關注。這些化合物以本身已知的方式藉使過量的上述藉由實例方式特定的類型之單純聚異氰酸酯類與具有對異氰酸酯基團有反應性之至少兩個基團之有機化合物(尤其是有機多羥基化合物)之反應而製備。這類型適合的多羥基化合物為分子量範圍為62至599(較佳地62至200)之單純多元醇類,例如乙二醇、三羥甲基丙烷、丙烷-1,2-二醇或丁烷-1,4-二醇或丁烷-2,3-二醇,而尤其是由聚胺基甲酸酯化學本身已知的這類型高分子量聚醚多醇類及/或聚酯多醇類,其具有分子量為600至12 000,較佳地
800至4000,及具有至少兩個(一般2至8,而較佳地2至6)一級及/或二級羥基基團。當然還可以使用彼等NCO預聚物,其(例如)係已獲自藉由實例方式特定的類型之較低分子量聚異氰酸酯類與具有對異氰酸酯基團有反應性之基團的次佳化合物,例如聚硫醚多醇類、具有羥基之聚縮醛類、多羥基聚碳酸酯類、具有羥基之聚酯醯胺類或含有羥基之烯烴性不飽和化合物之共聚物。
具有對異氰酸酯基團有反應性之基團(尤其是羥基)且適用於NCO預聚物製備之化合物為,例如,揭示於US-A 4 218 543之化合物。於該NCO預聚物製備中,這些具有對異氰酸酯基團有反應性之基團之化合物與上述藉由實例方式特定的類型之單純聚異氰酸酯類反應,同時維持NCO過量。該NCO預聚物一般具有NCO含量為10%至26%及較佳為15%至26%(以重量計)。由此已清楚的是,於本發明內文中,"NCO預聚物"及"具有終端異氰酸酯基之預聚物"據了解意指該反應產物及該含過量的未轉換的起始聚異氰酸酯類之混合物二者,其還經常係指為"半預聚物(semiprepolymer)"。
具有OH數為>500mg KOH/g之可用的脂族二醇包括常用於聚胺基甲酸酯化學之鏈延長劑(chain extender),諸如乙二醇、二乙二醇、丙二醇、二丙二醇、丁烷-1,4-二醇、丙烷-1,3-二醇。適宜為予以二醇類諸如2-丁烷-1,4-二醇、丁烷-1,3-二醇、丁烷-2,3-二醇及/或2-甲基丙烷-1,3-二醇。將理解的是以彼此的混合物形式使用脂族二醇類亦是可行的。
適合的H-活性成分為具有平均OH數為5至600mg KOH/g及平均官能度為2至6之多醇類。依照本發明適合的多醇類為,例如,多羥基聚醚類,其可獲自諸如乙二醇、二乙二醇、1,4-二羥基丁烷、1,6-二羥基己烷、二羥甲基丙烷、丙三醇、季戊四醇、山梨糖醇或蔗糖之適合起始劑分子之烷氧化反應。所用的起始劑同樣可為氨或胺類諸如乙二胺、己二胺、2,4-二胺基甲苯、苯胺或胺醇類或酚類(諸如雙酚A)。該烷氧化反應係使用環氧丙烷及/或環氧乙烷以任何所希望的順序或為一混合物之方式實行的。
以及多醇類,其對欲存在的至少一種交聯劑及/或鏈延長劑是另外可行的,係選自包含下述之胺類及胺醇類之組群,例如乙醇胺、二乙醇胺、二
異丙醇胺、乙二胺、三乙醇胺、異佛爾酮二胺、N,N’-二甲基(二乙基)乙二胺、2-胺基-2-甲基(或乙基)-1-丙醇、2-胺基-1-丁醇、3-胺基-1,2-丙烷二醇、2-胺基-2-甲基(乙基)-1,3-丙烷二醇,及醇類,例如乙二醇、二乙二醇、1,4-二羥基丁烷、1,6-二羥基己烷、二羥甲基丙烷、丙三醇及季戊四醇,還有山梨糖醇及蔗糖,或這些化合物之混合物。
還適合的是聚酯多醇類,其為可以本身已知方式藉使低分子量醇類與多元羧酸類(諸如己二酸、鄰苯二甲酸、六氫鄰苯二甲酸、四氫鄰苯二甲酸或這些酸的酸酐類)之反應而獲得,其條件為該H-活性成分之黏度不會變得過高。較佳的具有酯基團之多醇為蓖麻油(castor oil)。還另外適合的是包含蓖麻油之調配物,其如可藉樹脂(例如醛-酮樹脂)之溶解作用,及蓖麻油與以其它天然油為基底的多醇類之改質作用而獲得。
同樣適合的是彼等相當高分子量的多羥基聚醚類,其中高分子量聚加成物或聚縮合物或聚合物係以細微分散的、溶解的或接枝的形式存在。這類型改質的多羥基化合物可以本身已知的方式獲得,例如,當聚加成反應(e.g.於聚異氰酸酯類與胺基-官能性化合物之間的反應)或聚縮合反應(例如於甲醛與酚類及/或胺類之間的反應)時,可使得在具有羥基之化合物中原位進行。替代地,還可以混合一利用多羥基化合物之加工的水性聚合物分散液及之後將水自該混合物中移除。
藉乙烯基聚合物改質的多羥基化合物,如(例如)藉在聚醚類或聚碳酸酯多醇類存在下使苯乙烯與丙烯腈之聚合反應獲得,亦適用於聚胺基甲酸酯類之製備。當使用係已根據DE-A 2 442 101、DE-A 2 844 922及DE-A 2 646 141藉與乙烯基膦酸酯類及選擇性(甲基)丙烯腈、(甲基)丙烯醯胺或OH-官能性(甲基)丙烯系酯類之接枝聚合反應改質的聚醚多醇類時,可獲得卓越滯焰性之聚合物。
所述及的欲用作為H-活性化合物之代表性化合物敘述(例如)於High Polymers,Vol.XVI,“Polyurethanes Chemistry and Technology”,
Saunders-Frisch(ed.)Interscience Publishers,New York,London,vol.1,p.32-42,44,54及vol.II,1984,p.5-6及p.198-199。
使用所列舉化合物之混合物亦是可行的。
該H-活性成分之平均OH數及平均官能度之限制特別是源起於所產生的聚胺基甲酸酯之增加的脆性(embrittlement)。然而,原則上,此項技術領域熟悉者知悉影響該聚胺基甲酸酯之物理聚合物性質之方式,以使NCO成分、脂族二醇及多醇可以有利方式彼此互相配合。
該聚胺基甲酸酯層(b)可為發泡的或固體形式,例如為清漆或塗層形式。
可使用任何本身已知的輔助劑及添加劑製造,例如分離劑、發泡劑(blowing agent)、填充劑、催化劑及滯焰劑。
可選用的輔助劑及添加劑為:
a)水及/或揮發性無機或有機物質作為發泡劑
可用的有機發泡劑包括,例如,丙酮、乙酸乙酯、鹵素-取代的烷類,諸如二氯甲烷、氯仿、亞乙基氯化物、偏氯乙烯、單氟三氯甲烷、氯二氟甲烷、二氯二氟甲烷,還有丁烷、己烷、庚烷或二乙基醚,及可用的無機發泡劑包括空氣、CO2、或N2O。發泡效果還可透過添加在超過室溫之溫度下隨著氣體除去作用(例如氮氣除去作用)而分解的化合物而達成,實例為偶氮化合物諸如偶氮二甲醯胺(azodicarbonamide)及偶氮異丁腈(azoisobutyronitrile)。
b)催化劑
該催化劑為,例如,三級胺類(諸如三乙基胺、三丁基胺、N-甲基嗎啉、N-乙基嗎啉、N,N,N’,N’-四甲基乙二胺、五甲基二伸乙基三胺及更高級的同系物、1,4-二氮雜雙環[2.2.2]辛烷、N-甲基-N’-二甲基胺基乙基哌嗪、雙(二
甲基胺基烷基)哌嗪類、N,N-二甲基苄基胺、N,N-二甲基環己基胺、N,N-二乙基苄基胺、雙{N,N-二乙基胺基乙基)己二酸酯、N,N,N’,N’-四甲基-1,3-丁烷二胺、N,N-二甲基-β-苯基乙基胺、1,2-二甲基-咪唑、2-甲基咪唑)、單環系及雙環系醯胺類、雙(二烷基胺基)烷基醚類、具有醯胺基團(較佳地甲醯胺基團)之三級胺類、形成自二級胺類(諸如二甲基胺)與醛類(較佳地甲醛)或酮(諸如丙酮、甲基乙基酮或環己酮)及酚類(諸如酚、壬基酚或雙酚)之Mannich鹼、具有對異氰酸酯基團有活性之氫原子之三級胺(e.g.三乙醇胺、三異丙醇胺、N-甲基二乙醇胺、N-乙基二乙醇胺、N,N-二甲基乙醇胺),及其與環氧烷類(諸如環氧丙烷及/或環氧乙烷)之反應產物,二級/三級胺類,具有碳-矽鍵之矽胺類(silaamines)(2,2,4-三甲基-2-矽嗎啉及1,3-二乙基胺基甲基四甲基二矽氧烷),含有氮之鹼(諸如四烷基銨氫氧化物),鹼金屬氫氧化物(諸如氫氧化鈉),鹼金屬苯氧化物(諸如苯氧化鈉),鹼金屬烷氧化物(諸如甲氧化鈉),及/或六氫三嗪類(hexahydrotriazines)。
利用於該內醯胺與該具有酸性氫之化合物之間結合之初始形成作用,於NCO基團與Zerewitinoff-活性氫原子之間的反應,係以本身已知的方式,還藉內醯胺類(lactams)與氮雜內醯胺類(azalactams)大幅度地加速。
使用有機金屬化合物作為催化劑亦是可行的,尤其是有機錫及/或鉍化合物。可用的有機錫化合物包括,以及硫化合物諸如二-n-辛基錫硫醇鹽(octyltin mercaptide),較佳地羧酸之錫(I1)鹽諸如乙酸錫(II)、辛酸錫(II)、乙基己酸錫(II)及月桂酸錫(II),及錫(IV)化合物,例如氧化二丁基錫、二氯化二丁基錫、二乙酸二丁基錫、二月桂酸二丁基錫、馬來酸二丁基錫或二乙酸二辛基錫。有機鉍催化劑敘述(例如)於專利申請案WO 2004/000905。
當然可以使用上述提及的任何催化劑作為混合物。於本內文中特別受關注的是有機金屬化合物與脒類(amidines)、胺基吡啶類或肼基吡啶類(hydrazinopyridines)之組合。
該催化劑一般以約0.001%至10%(以重量計)之用量使用,以具有對異氰
酸酯有反應性之至少兩個氫原子之化合物之總用量為基準。
c)表面-活性添加劑諸如乳化劑及發泡體穩定劑
可用的乳化劑包括,例如,蓖麻油磺酸鹽之鈉鹽或脂肪酸與胺類之鹽類,諸如油酸二乙基銨鹽或硬脂酸二乙醇銨鹽。使用磺酸之鹼金屬或銨鹽作為表面-活性添加劑亦是可行的,例如十二烷基苯磺酸或二萘基甲烷二磺酸,或脂肪酸(諸如蓖麻油酸(ricinoleic acid))或聚合性脂肪酸之鹼金屬或銨鹽。
可用的發泡體穩定劑包括特別是聚醚矽氧烷類,尤其是水溶性代表物。這些化合物之結構一般使得一環氧乙烷與環氧丙烷之共聚物鍵結至聚二甲基矽氧烷自由基。特別關注的是具經由脲甲酸酯基之多重支化(multiple branching)之聚矽氧烷-聚氧伸烷基共聚物。
d)反應延遲劑
可用的反應延遲劑包括,例如,酸性物質(諸如氫氯酸或有機酸鹵化物)。
e)添加劑
可用的PU添加劑包括,例如,本身已知類型的單元調節劑(cell regulator)(諸如石蠟類或脂肪醇類)或二甲基聚矽氧烷類,還有顏料或染料及本身已知類型的滯焰劑(例如參(氯乙基)磷酸酯、三甲酚基磷酸酯或磷酸銨及聚磷酸酯),還有對抗老化及風化影響之穩定劑、塑化劑及抑菌性(fungistatic)與制菌性(bacteriostatic)物質,還有填充劑(諸如硫酸鋇、矽藻土(kieselguhr)、碳黑或沉澱性白堊(precipitated chalk))。
依照本發明任選的另外用途,表面-活性添加劑及發泡體穩定劑,還有單元調節劑、反應延遲劑、穩定劑、滯焰性物質、塑化劑、染料及填充劑,還有抑菌性與制菌性物質之其它實例為此項技術領域熟悉者已知的及敘述於文獻中。
實施例
成分A
以雙酚A為基底之線性聚碳酸酯,具有重量平均分子量Mw為28 000g/mol。
成分B-1
聚對苯二甲酸丁二酯,具有一熔體流動速率(MFR)為49.0g/10min,依DIN EN ISO 1133在250℃下以2.16kg荷重測得。
成分B-2
聚對苯二甲酸丁二酯,具有一熔體流動速率(MFR)為12.0g/10min,依DIN EN ISO 1133在250℃下以2.16kg荷重測得。
成分C
ABS聚合物,在72重量%(以ABS聚合物為基準)的粒狀交聯的聚丁二烯橡膠(中值粒子直徑d50=0.36μm)之存在下,藉使28重量%(以ABS聚合物為基準)之24重量%丙烯腈與76重量%苯乙烯之混合物的乳化聚合反應而製備的。
成分D-1
具有下述構造單元之寡聚性亞磷酸酯穩定劑
成分D-2
檸檬酸,可商業上獲自Hamann und Reimer。
成分D-3
雙(2-羥基-3-環己基-5-甲基苯基)甲烷之亞磷酸酯,可商業上獲自如Rhein Chemie Rheinau GmbH之Addovate ThermoStab品名。
成分D-4
四硬脂酸酯季戊四醇酯,可商業上獲自如Emery Oleochemicals之Loxiol VPG 861。
成分D-5
以褐煤酯(montanic ester)為基底的蠟,可商業上獲自Clariant International Ltd之Licowax E trade品名。
成分D-6
Naintsch A3c:超微細研磨的高純度滑石,得自Naintsch Mineralwerke GmbH(Graz,Austria)。
成分D-7
黑色顏料Black Pearls 800,可商業上獲自Cabot Corporation。
反應性聚胺基甲酸酯塗層系統
所用的聚胺基甲酸酯塗層系統為一Desmophen® XP 2488(多醇成分)與
Desmodur® N3600(聚異氰酸酯成分)之混合物,兩者均得自Bayer MaterialScience AG, Leverkusen,Germany,以1:1.7重量份之混合比例。
Desmophen® XP 2488為分支的聚酯多醇,具有依DIN 53019在20℃下13 250 mPa.s之黏度,依DIN 51757在20℃下1.12g/cm3之密度,及16.0%之OH含量。
Desmodur® N3600為以六亞甲基二異氰酸酯為基底的脂族異氰酸酯,具有依DIN EN ISO 11909之NCO含量為23.5重量%,依DIN EN ISO 3219/A.3在23℃下1200mPa.s之黏度,及依DIN EN ISO 2811在20℃下1.16g/cm3之密度。
該聚胺基甲酸酯塗層系統之交聯係以可商業上獲自OMG Borchers GmbH,Langenfeld之二月桂酸二丁基錫(DBTL)催化。所添加的量為0.5重量份,以多醇成分與聚異氰酸酯成分之總和為基準。
該聚碳酸酯模塑組成物之製造及特性化
於一雙螺桿擠壓機(twin-screw extruder)(ZSK-25)(得自Werner and Pfleiderer)中,列示於表1之原料在220rpm速度下與在260至280℃範圍之熔融溫度下以20kg/h通量(throughput)被摻合及在該化合物熔體冷卻與固化之後被粒化。
產生自該特定摻合操作之顆粒係以注射模塑機(得自Arburg)在260℃熔融溫度下與80℃模塑溫度下製得,以得到尺寸80mm x 10mm x 4mm之試驗樣品。
除非另有說明,特定於本申請案中的參數藉下述方法測定:
該模塑組成物之延展性(ductility),使用依ISO 180-1A在-30℃下在這些
試驗樣品上測得的耐缺口衝擊性值ak評估。
耐熱變形性,使用依ISO 306在這些試驗樣品上測得的Vicat B120值評估。
在斷裂時伸長率,依ISO 527-1,-2之拉伸試驗以50mm/min之延伸速率測量。
彈性之模量,依ISO 527-1,-2之拉伸試驗以1mm/min之延伸速率測量。
總收縮率(total shrinkage),使用具有尺寸150mm*105mm*3mm之試樣於以ISO 2577為基礎之方法測定。該試樣,在260℃熔融溫度下、70℃模塑溫度下及600巴保持壓力下製造。樣品在空氣循環烘箱中90℃下調節1小時之後,測定該數值。
於該由聚碳酸酯組成物構成的基材與該聚胺基甲酸酯皮之間的複合體黏著性,係在具有20mm寬度之條狀樣品(其由此製得的部分PU-塗布的2-成分複合片部分鋸出)上,依DIN EN 1464藉浮動輥試驗(floating roller test)以100mm/min之試驗速度測定。該複合體黏著性,於溫度變化試驗中(TVT)(1st循環:在105℃下15小時,接著在30℃下30分鐘,接著在-40℃下8小時,接著在23℃下30分鐘),在樣品老化3或6日之後測定。
複合組件之製造
具有412cm2之突出區域(projected area)之部分表面-塗布的模塑體以注射模塑機於具有二個空穴(一基材-面空穴與一被連接至RIM系統之聚胺基甲酸酯-面塗層空穴)之注射模塑體中製造。該複合組件為由熱塑性聚合物(載體)所構成之片狀組件,其表面係已經被部分塗布有聚胺基甲酸酯層。該載體模塑之璧厚度為約4mm。該聚胺基甲酸酯層厚度為200μm。
為更佳描述,敘述於實施例之根據本發明用於製造本發明複合組件之方法示於圖1。
於第一方法步驟中,製造該載體模塑體。為這目的,如表1所述的組成物之熱塑性聚合物顆粒係於射出-模塑筒(injection-moulding barrel)中熔融及在270℃溫度下注入該閉合的模塑體之第一模塑體空穴內(於圖1之步驟1及2)。將這模塑體空穴加熱至80℃之溫度。在保持-壓力時間及冷卻時間之後,其導致該載體之固化作用,隨時間過去,於第二方法步驟中開啟該模塑體(於圖1之步驟3)。完成此,係藉保持該注射模塑體之推出器面(ejector side)上製得的載體組件及從該載體位置(於圖1之步驟3)連同該模塑體核芯使用一滑桿(slider)將它一起移動至該塗布位置內(於圖1之步驟4)。其後,再度閉合該注射模塑體(於圖1之步驟5),施予一最大壓力200巴之夾持力(clamping force)及,於第三方法步驟中,在約30巴壓力下將該不含溶劑之反應性聚胺基甲酸酯系統(見上述)注入該塗布空穴內(於圖1之步驟6)。完成此,係藉將該聚胺基甲酸酯塗層系統之二個反應性成分從該RIM系統輸送至高壓逆流混合頭(high-pressure countercurrent mixing head)內及在注射之前於其中混合它們。將該PU-面空穴加熱至80℃溫度。在注射結束後,為了避免該塗層材料之回流(backflow),該聚胺基甲酸酯混合頭之注射噴嘴(injection nozzle)藉由液壓筒(hydraulic cylinder)之方式在50巴壓力下先予密封。在反應及冷卻時間過後,於第四方法步驟中,再次開啟該模塑體(於圖1之步驟7)及將該塗布的模塑體脫模(於圖1之步驟8)。
由表1顯而易見,本發明實施例1至4展現不僅僅在溫度變化試驗後對該聚胺基甲酸酯系統之黏著性上明顯改良,而且有持續高的或改良的韌性、高的耐熱變形性、高的斷裂時伸長率與高的彈性之模量及良好平衡的收縮特性。性質之最適組合只當該聚丁二烯含量以成分A+B+C為基準落在本發明範圍內時達成及,同時,不含丁二烯的乙烯基(共)聚合物之含量同樣落在本發明範圍內。如比較例1及3,若該聚丁二烯含量及該不含丁二烯的乙烯基(共)聚合物含量均過低時,該黏著性不會到達產業上所要求的程度。更且,耐缺口衝擊性明顯下降。如比較例2,若該聚丁二烯含量過高時,該整體收縮率無法滿足技術上可接受程度。特佳的模塑組成物為彼等對其整體收縮率不會超過1.28%及同時在溫度變化試驗持續6日之後該組成物黏著性為>7N/mm。
Claims (15)
- 一種組成物,包含A)30至45重量份的至少一種聚合物,選自包括芳香族聚碳酸酯與芳香族聚酯碳酸酯之構成組群,B)32至54重量份的至少一種聚對苯二甲酸伸烷基酯,較佳為聚對苯二甲酸丁二酯,C)16至23重量份的至少一種混合物,包含至少一種聚丁二烯系接枝聚合物與至少一種不含丁二烯的乙烯基(共)聚合物,D)0.1至20.0重量份(以於各情況下成分A至C之總和為基準)的至少一種聚合物添加劑,於此,該聚丁二烯含量以成分A至C之重量份總和為基準為8%至18%(以重量計),及於此,來自成分C之不含丁二烯的乙烯基(共)聚合物之總含量以成分A至C之重量份總和為基準為3%至12%(以重量計),及於此,在該聚碳酸酯組成物中的成分A至C之重量份總和被標定至100。
- 根據申請專利範圍第1項之組成物,包含A)32至45重量份的至少一種聚合物,選自包括芳香族聚碳酸酯與芳香族聚酯碳酸酯之構成組群,B)32至50重量份的至少一種聚對苯二甲酸伸烷基酯,較佳為聚對苯二甲酸丁二酯,C)17至22重量份的至少一種混合物,包含至少一種聚丁二烯系接枝聚合物與至少一種不含丁二烯的乙烯基(共)聚合物,D)0.2至15.0重量份(以於各情況下成分A至C之總和為基準)的至少一種聚合物添加劑,於此,該聚丁二烯含量以成分A至C之重量份總和為基準為9%至17%(以重量計),及於此,來自成分C之不含丁二烯的乙烯基(共)聚合物之總含量以成分A至C之重量份總和為基準為4%至11%(以重量計),及於此,在該聚碳酸酯組成物中的成分A至C之重量份總和被標定至100。
- 根據申請專利範圍第1項之組成物,包含A)35至45重量份的至少一種聚合物,選自包括芳香族聚碳酸酯與芳香族聚酯碳酸酯之構成組群,B)32至45重量份的至少一種聚對苯二甲酸伸烷基酯,較佳地為聚對苯二甲酸丁二酯,C)18至21重量份的至少一種混合物,包含至少一種聚丁二烯系接枝聚合物與至少一種不含丁二烯的乙烯基(共)聚合物,D)0.3至10.0重量份(以於各情況下成分A至C之總和為基準)的至少一種聚合物添加劑,於此ㄝ該聚丁二烯含量以成分A至C之重量份總和為基準為10%至16%(以重量計),及於此,來自成分C之不含丁二烯的乙烯基(共)聚合物之總含量以成分A至C之重量份總和為基準為5%至10%(以重量計),及於此,在該聚碳酸酯組成物中的成分A至C之重量份總和被標定至100。
- 根據前述申請專利範圍中一項之組成物,其中成分C包含C.1 5%至60%,較佳地15%至58%及尤其是20%至55%(以重量計)的至少一種乙烯基單體,以成分C.1為基準,在C.2 95%至40%,較佳地85%至42%及尤其是80%至45%(以重量計)的一或多種聚丁二烯系接枝基質上,以成分C.1為基準。
- 根據申請專利範圍第4項之組成物,其中成分C.1包含下述之混合物C.1.1 50至99重量份的乙烯基芳香族化合物及/或環-取代的乙烯基芳香族化合物(諸如苯乙烯、α-甲基苯乙烯、p-甲基苯乙烯、p-氯苯乙烯)及/或甲基丙烯酸(C1-C8)-烷基酯(諸如甲基丙烯酸甲基酯、甲基丙烯酸乙基酯),以C.1為基準,及C.1.2 1至50重量份的乙烯基氰化物(不飽和腈類諸如丙烯腈及甲基丙烯腈) 及/或(甲基)丙烯酸(C1-C8)-烷基酯(諸如甲基丙烯酸甲基酯、丙烯酸n-丁基酯、丙烯酸t-丁基酯),及/或不飽和羧酸之衍生物(諸如酸酐類及醯亞胺類),例如順丁烯二酸酐及N-苯基馬來醯亞胺,以C.1為基準。
- 根據前述申請專利範圍中一或多項之組成物,其中成分D包含熱穩定劑、脫模劑、色料及UV吸收劑。
- 根據前述申請專利範圍中一或多項之組成物,其中成分B為聚對苯二甲酸丁二酯。
- 一種複合組件,包含a)一載體,由根據申請專利範圍第1至7項中一或多項之熱塑性塑膠組成物所構成b)至少一種聚胺基甲酸酯層,得自包括塗層材料、發泡體及壓實皮之組群,包含- 至少一種聚異氰酸酯成分,- 至少一種多官能性H-活性化合物,及- 選擇地至少一種聚胺基甲酸酯添加劑及/或加工助劑,及特徵為NCO-對H-活性基團之莫耳比為1:1至1.1:1。
- 根據申請專利範圍第8項之複合組件,其中該聚胺基甲酸酯層為一具有層厚度為50至300μm之塗層材料.
- 根據申請專利範圍第8項之複合組件,其中該聚胺基甲酸酯層為一具有層厚度為1mm至1cm之發泡體。
- 根據申請專利範圍第8項之複合組件,其中該聚胺基甲酸酯層為一具有層厚度為1mm至4mm之壓實皮。
- 一種製造根據前述申請專利範圍中任一項之複合組件之方法,其特徵在於該聚胺基甲酸酯層係已藉反應性聚胺基甲酸酯原料混合物之完全聚合反 應製備的,該混合物包含- 至少一種聚異氰酸酯成分,- 至少一種多官能性H-活性化合物,及- 選擇地至少一種聚胺基甲酸酯添加劑及/或加工助劑,其係與該已事先成形自該熱塑性塑膠組成物及固化的載體直接接觸。
- 一種製造根據前述申請專利範圍中任一項之複合組件之方法,其特徵在於(i)於第一方法步驟,將該熱塑性塑膠組成物之熔體注入一第一模塑體空穴內及之後冷卻,(ii)於第二方法步驟,將該冷卻的熱塑性塑膠成分移入一較大的空穴內及藉此製得一界定的間隙,(iii)於第三方法步驟,於該熱塑性塑膠成分與該擴大的空穴之模塑體表面之間所形成的間隙內注入有一反應性聚胺基甲酸酯原料混合物,其包含- 至少一種聚異氰酸酯成分,- 至少一種多官能性H-活性化合物,及- 選擇地至少一種聚胺基甲酸酯添加劑及/或加工助劑,係與該熱塑性塑膠載體表面直接接觸而使該聚胺基甲酸酯原料混合物完全聚合,以得到一壓實聚胺基甲酸酯層或得到一聚胺基甲酸酯發泡體層,(iv)於第四方法步驟,將該複合組件從該模塑體空穴中脫模,方法步驟(i)至(iv)係彼此接著立即連續進行。
- 根據申請專利範圍第13項之方法,特徵在於方法步驟(iii)中,該與熱塑性塑膠組成物接觸之注射模塑體之表面被加熱至60至90℃範圍之溫度,及該與反應性聚胺基甲酸酯混合物接觸之注射模塑體之表面被加熱至60至90℃範圍之溫度。
- 一種根據申請專利範圍第8至11項中任一項之複合組件之用途,係用作為鐵路車輛、飛機或汽車之內部或外部組件及電氣/電子組件之內部或外部組件。
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