TW201341186A - 防止缺陷之隔音聚合物內層 - Google Patents
防止缺陷之隔音聚合物內層 Download PDFInfo
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- TW201341186A TW201341186A TW102108416A TW102108416A TW201341186A TW 201341186 A TW201341186 A TW 201341186A TW 102108416 A TW102108416 A TW 102108416A TW 102108416 A TW102108416 A TW 102108416A TW 201341186 A TW201341186 A TW 201341186A
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- polymer layer
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Abstract
本發明係關於用於多層玻璃板之聚合物內層及具有至少一聚合物內層片之多層玻璃板之領域。具體言之,本發明係關於包含防止形成光學缺陷之多個熱塑性層之聚合物內層之領域。
Description
本申請案主張2012年3月9日申請之美國臨時申請案第61/609092號之優先權,該案係以引用全文之方式併入本文。
本發明係關於用於多層玻璃板之聚合物內層及具有至少一聚合物內層片之多層玻璃板之領域。具體言之,本發明係關於包含防止形成光學缺陷之多個熱塑性層之聚合物內層之領域。
圖1描繪在三層式內層中之氣泡發起及膨脹。
圖2描繪常見於具有多層內層之玻璃板中之缺陷之實例。
圖3描繪根據冰花測試形成於聚對苯二甲酸乙二酯(PET)膜中之冰花之實例。
圖4描繪在習知多層內層層壓板中之彎曲應力及在本發明內層中之此種應力的下降。
本發明係關於用於多層玻璃板之聚合物內層及具有至少一聚合物內層片之多層玻璃板之領域。具體言之,本發明係關於包含防止形成光學缺陷之多個熱塑性層之聚合物內層之領域。
一般而言,多層玻璃板係指包含夾在兩玻璃板之間之內層之層
壓板。層壓多層玻璃板常用於建築門窗應用及車輛與飛機之窗體中。此等應用常稱為層壓安全玻璃。在層壓安全玻璃中之內層之主要功能係吸收由於衝擊或施加至玻璃之力所導致之能量、保持玻璃之層黏合(甚至當施加力及玻璃破裂時),及防止玻璃破裂成尖銳碎片。此外,內層一般使玻璃具有遠更高之聲音隔絕評級、降低UV及/或IR光透射、及增強相關窗體之美觀性。
為使玻璃板獲得所需及最優的聲音隔絕,一般實務係利用具有夾在兩較硬「皮」層之間之至少一軟「芯」層之多層內層。內層之此等層一般係透過將聚合物樹脂(如聚(乙烯醇縮丁醛)與一或多種塑化劑混合及藉由任何適用方法或熟習本項技術者已知之方法(包括,但不限於,擠壓)將該混合物熔化加工成片材而製成,然後藉由諸如共擠壓及層壓之方法組合該等層。可針對各種其他目的視需要添加其他額外成分。在形成內層片後,一般將其收集並捲起用於運輸及儲存並隨後用於如下文所述之多層玻璃板中。
下文提供一般製造與隔音內層組合之多層玻璃板之方式的簡化描述。首先,將多層內層放置在兩基板之間及自邊緣修整任何多餘內層,藉此形成組合件。隨後,藉由適用方法或熟習本項技術者已知之方法(例如,藉由軋輥、真空袋或另一脫氣機制)將空氣自組合件移除。此外,藉由本技藝一般熟練者已知之任何方法將內層部分壓黏至基板。為形成最終一體式結構,隨後藉由本技藝一般熟練者已知之高溫高壓層壓方法(如,但不限於,高壓釜處理)使該初步黏合更為持久。
含有此等多層隔音內層之玻璃板會在極端條件下產生通常稱為冰花(亦稱為雪片)之缺陷,該等缺陷係由過量殘餘物之存在、內層中之截留空氣及玻璃中之應力所引起。具體言之,在層壓多層玻璃板結構之製造過程期間,當將此等層堆疊在一起以形成多層內層時,空
氣及其他氣體經常會截留在基板與內層之間或多層內層之個別層之間的間隙空間中。如上所述,此截留空氣一般於上釉或板製造過程中藉由真空或軋輥除去結構空氣之方式來移除。然而,此等技術並非始終能有效地移除截留在基板之間之間隙空間中之全部空氣。此等空氣缺口在失配玻璃(例如,回火玻璃、熱強化玻璃及厚退火玻璃)及擋風玻璃(其中玻璃之曲率一般導致氣隙)中尤其明顯。在擋風玻璃中之此等氣隙常稱為「彎曲間隙」。此外,當在高壓釜處理期間存在彎曲間隙時,熱及壓力壓縮玻璃以順應內層及縮窄該間隙,導致在玻璃之原間隙區域中產生高應力。
如上所述,除氣技術無法始終有效地將全部空氣自玻璃板組合件移除。因此,在玻璃與內層之間存在殘留空氣。在高壓釜處理期間,在熱及壓力下,殘留空氣溶解至內層中(大部分在皮層中)。位於皮層中之殘留空氣可移動至芯層或皮-芯界面中,及最終分配在皮層與芯層之間以達到平衡狀態。當大量殘留空氣(例如,過量殘留空氣)存在於內層中時,氣泡可成核,尤其在高溫下,係因內層變軟且變得難以阻止成核。
就習知隔音內層而言,氣泡通常首先形成於軟芯層內,係因成核趨於在較低黏度介質中發生。在溫熱氣候中,如在夏季期間,安裝在建築物及車輛上之層壓玻璃中之玻璃之溫度可升高至50℃至100℃。在此等升高之溫度下,由玻璃板或擋風玻璃中之應力所產生之力在玻璃上垂直於其等平面及沿相反方向施加壓力,進而將玻璃板彼此牽離以試圖恢復其等原始狀態。應力使空氣成核及膨脹的抗性降低並容許氣泡在芯層內生長。
圖1描繪在三層式內層中氣泡之發起及膨脹。不論氣泡在何處開始形成,在升高之溫度(例如,50℃至100℃)下,源自彎曲間隙或玻璃失配之應力導致氣泡在芯層中沿隨機徑向方向中之最小抗性路徑
膨脹。隨著缺陷繼續徑向膨脹,形成分支及樹枝狀特徵,且展現不適宜之冰花光學外觀。形成於安裝擋風玻璃中之此種缺陷之一實例出示在圖2中。此外,冰花在芯層內之形成一般會導致層分離,進而降低板之結構完整性。
因此,本技藝需要開發一種防止此等光學缺陷形成,而不使習知多層內層之其他光學、機械及聲學特性下降之多層內層。更具體言之,本技藝需要開發減小玻璃中之應力及容許在玻璃板製造期間移除空氣之多層內層。
由於本文中所描述之在本技藝中之此等及其他問題,故尤其提供一種多層內層,其包含透過改變層之分子量及組成而形成之具有不同流變性質之層。在一實施例中,此等多層內層包含:第一聚合物層,其包含具有小於約140,000道爾頓之分子量之塑化聚(乙烯醇縮丁醛);第二聚合物層,其包含具有大於約140,000道爾頓之分子量之塑化聚(乙烯醇縮丁醛);及第三聚合物層,其包含具有小於約140,000道爾頓之分子量之塑化聚(乙烯醇縮丁醛)。第二聚合物層係佈置在第一聚合物層與第三聚合物層之間,形成兩個皮層及一中央芯層。
使用本發明之具有較低分子量之皮層容許內層在高壓釜處理溫度下之流動增加而不折損習知多層內層之其他有利/所需特性。換言之,使用本發明之具有較低分子量之皮層影響其等在高壓釜處理期間之流動,同時維持如透過聲音傳輸損失、光學性質、機械強度及抗衝擊性所測量之習知多層內層之所有其他特性。類似地,可操縱塑化劑負載、兩或更多種塑化劑之混合物、殘餘羥基含量或該三種性質之任何組合或平衡,以進一步輔助獲得高流動皮層。因此,可透過以高流動皮層部分填充間隙區域,來減小擋風玻璃及層壓玻璃組合件中所固有之應力值,藉此減少多層內層常見之光學缺陷。
此外,多層內層之表面可經壓紋以產生用於在除氣過程期間使空氣逸出之一致表面粗糙度及通道;藉此顯著降低可用於氣泡成核及膨脹之空氣量,進而進一步減少缺陷。
適宜地,本發明內層有效減少或消除因彎曲多層板而導致之截留空氣及間隙及應力(在本文中共同稱為「彎曲間隙」),同時仍維持習知多層內層之聲學及光學性質。由於多層板中所固有之截留空氣及彎曲間隙經減少,故亦藉此減少或消除諸如冰花(或雪片)之光學缺陷之形成。
為利於更好地理解本文中所揭示之包含高流動皮層之內層,本申請案首先提供一些定義術語、製造方法之概述及內層(包括一般性及於本發明內層中)中所包含之常見組份之概述、以及其等之形成,然後再討論將高流動皮層併入至內層中以減少光學缺陷之形成。
如本文中所使用之術語「聚合物內層片」、「內層」及「聚合物熔化片」可指單層片或多層內層。正如其名,「單層片」係經擠壓成一個層之單個聚合物層。另一方面,多層內層可包含多個層,包括分開擠壓之層、共擠壓層或分開與共擠壓層之任何組合。因此,多層內層可包含,例如:組合在一起之兩或更多個單層片(「複層片」);一起共擠壓之兩或更多個層(「共擠壓片」);組合在一起之兩或更多個共擠壓片;至少一單層片與至少一共擠壓片之組合;及至少一複層片與至少一共擠壓片之組合。在本發明之各種實施例中,多層內層包含經佈置成彼此直接接觸之至少兩聚合物層(例如,單層或共擠壓之多層),其中各層包含如下文更完整詳細說明之聚合物樹脂。就此而言,如本文中所使用之「皮層」一般係指內層之外部層及「芯層」一般係指內部層。因此,一示例性實施例將係:皮層//芯層//皮層。然而,應注意,其他實施例包括具有多於三個層(例如,4、5、6或至多10個個別層)之內層。
此外,涵蓋如本文中所描述之聚合物內層片可藉由本技藝一般熟練者已知之製造可用於多層板中之聚合物內層片的任何合適方法製造。例如,涵蓋可透過溶液澆鑄、壓縮模製、射出成型、熔化擠壓、共擠壓、熔化吹製或用於生產及製造本技藝一般熟練者已知之聚合物內層片之任何其他製程形成聚合物內層片。此外,在使用多個聚合物內層之實施例中,涵蓋此等多個聚合物內層可透過共擠壓、吹膜、浸塗、溶液塗佈、刮刀、槳片、空氣刀、印刷、粉末塗佈、噴塗或本技藝一般熟練者已知之其他方法形成。
最終內層,不論係由擠壓或共擠壓形成,一般具有隨機粗糙表面形態,因其係於離開擠壓模具時透過聚合物熔體之熔化破裂形成且可額外地在一或兩側(例如,皮層)之隨機粗糙表面上藉由本技藝一般熟練者已知之任何壓紋方法進行壓紋。此種壓紋方法之一實例揭示於美國專利案第4,671,913號中(該案以引用全文之方式併入本文)。壓紋使聚合物內層之表面上形成微小凸起及凹陷部分,經顯示該等部分可有效增進除氣過程及減少氣泡之發生。例如,現已發現在100℃下加熱5分鐘後,具有25至50微米之表面粗糙度(Rz)之壓紋內層極其良好地在軋輥及真空除氣中工作,且當與未壓紋內層比較時,展示優異的冰花缺陷形成抗性。在本發明之其他實施例中,在100℃下加熱5分鐘後之表面粗糙度(Rz)之範圍可為25至66微米、25至60微米、及25至65微米。
可藉由操縱層之組成、厚度或位置及類似參數來改變任何多層內層。因此,涵蓋多層內層片之皮層及芯層可包含相同熱塑性材料或不同熱塑性材料。典型聚合物包括,但不限於,聚(乙烯醇縮丁醛)(PVB)、聚胺基甲酸酯、聚氯乙烯、聚(乙烯-共-乙酸乙烯酯)、上述聚合物之組合及類似物。PVB、聚氯乙烯及聚胺基甲酸酯一般為內層之較佳聚合物;PVB為特佳。例如,多層內層可由作為皮層之PVB及
作為芯層之聚氯乙烯或聚胺基甲酸酯組成。其他實例包括以聚氯乙烯或聚胺基甲酸酯作為皮層及以PVB作為芯層。或者,皮層及芯層可均為使用相同或不同起始樹脂之PVB。
可將各種黏著控制劑(ACA)用於本發明之內層中。內層調配物中之ACA控制片材對玻璃之黏著,以在玻璃層壓板受衝擊時提供能量吸收。在本發明之內層之各種實施例中,內層可包含約0.003至約0.15份ACA/100份樹脂;約0.01至約0.10份ACA/100份樹脂;及約0.01至約0.04份ACA/100份樹脂。此種ACA包括,但不限於,美國專利案第5,728,472號(該案以引用全文之方式併入本文)中所揭示之ACA、殘餘乙酸鈉、乙酸鉀、雙(2-乙基丁酸)鎂及/或雙(2-乙基己酸)鎂。
可將其他添加劑併入至內層中,以增強其於最終產品中之性能及賦予內層某些額外性質。在一般技術者已知之其他添加劑中,此等添加劑包括,但不限於,染料、顏料、穩定劑(例如,紫外線穩定劑)、抗氧化劑、抗阻斷劑、阻燃劑、IR吸收劑或阻斷劑(例如,氧化銦錫、氧化銻錫、六硼化鑭(LaB6)及氧化銫鎢)、加工助劑、流動增強添加劑、潤滑劑、衝擊改質劑、成核劑、熱穩定劑、UV吸收劑、UV穩定劑、分散劑、表面活性劑、螯合劑、偶合劑、黏著劑、底劑、強化添加劑及填充劑。
在本發明之內層之各種實施例中,內層將包含約30至約60 phr(份/百份樹脂)之總塑化劑。雖然上文指出總塑化劑含量,然而在皮層或芯層中之塑化劑含量可不同於總塑化劑含量。此外,皮層及芯層可具有不同塑化劑含量,係因在平衡態時各別層之塑化劑含量係由其各別殘餘羥基含量決定,如美國專利案第7,510,771號(該案係以引用全文之方式併入本文)所揭示。例如,當組合皮層厚度等於芯層厚度時,針對約54.3 phr之內層之總塑化劑量,在平衡時,內層可包含各具有38 phr塑化劑之兩皮層,及具有75 phr塑化劑之芯層。就較厚
或較薄皮層而言,內層之總塑化劑量將相應地變化。
可在高壓釜處理溫度下透過適當選擇塑化劑之類型來增大皮層之流動。在環境溫度下與熱塑性聚合物(如PVB)較不相容之塑化劑需要高負載量來達成習知多層內層之特性。然而,此等高負載塑化劑在高溫下可變得較相容,導致高壓釜處理流動增大,此係因高塑化劑負載量增大聚合物鏈之「自由體積」。此種較不相容的塑化劑包括,但不限於,較高分子量塑化劑,如聚合塑化劑(具有小於2,000道爾頓之分子量之聚己二酸酯)、大豆油及環氧化大豆油。亦可使用具有不同相容性之兩或更多種塑化劑之混合物以增大皮層之高壓釜處理流動。皮層一般將包含約30至約55 phr塑化劑,更佳約35至約50 phr,而不影響習知多層內層之特性。當然,可針對適用於特定應用而使用其他量。
在一些實施例中,習知塑化劑具有少於20、少於15、少於12或少於10個碳原子之烴鏈段。用於此等內層中之合適習知塑化劑尤其包括多元酸或多元醇之酯。合適塑化劑包括,例如,二-(2-乙基己酸)三乙二醇酯(3-GEH)、二-(2-乙基己酸)四乙二醇酯、二-(2-乙基丁酸)三乙二醇酯、二庚酸三乙二醇酯、二庚酸四乙二醇酯、己二酸二己酯、己二酸二辛酯、環己基己二酸己酯、己二酸二異壬酯、己二酸庚基壬酯、癸二酸二丁酯、聚合己二酸酯、大豆油及環氧化大豆油、及其等混合物。更佳的塑化劑係3-GEH。此外,較佳可使用在高溫下相容之塑化劑以進一步增大內層之流動。
如本文中所使用,塑化劑或內層中之任何其他組分之量可以份/百份樹脂(phr)重量比測量。例如,若將30克塑化劑添加至100克聚合物樹脂,則所得塑化聚合物之塑化劑含量將為30 phr。如本文中所使用,當給定內層之塑化劑含量時,參照用於產生該內層之熔化物中之塑化劑之phr來確定塑化劑含量。
塑化劑透過使自身包埋在聚合物鏈之間,分開該等聚合物鏈(增大「自由體積」)及藉此顯著降低聚合物樹脂之玻璃轉變溫度(Tg)(一般達0.5至4℃/phr),進而使材料變軟來起作用。就此而言,可調節內層中之塑化劑之量以影響玻璃轉變溫度(Tg)。玻璃轉變溫度(Tg)係標記內層自玻璃態轉變為橡膠態之溫度。一般而言,較高塑化劑負載量將產生較低Tg。先前使用之習知內層一般具有在約0℃(針對隔音(降噪)內層)至約45℃(針對颶風及飛機內層應用)範圍內之Tg。
玻璃轉變溫度(Tg)係藉由動態機械分析(DMA)確定。DMA測量儲存(彈性)模量(G’)(帕斯卡)、損失(黏性)模量(G”)(帕斯卡)、作為在給定頻率、及溫度掃描速率下之溫度之函數之試樣的損失(阻尼)因數(LF)[tan(△)]。當樣品溫度在2℃/分鐘之速率下自-20℃升高至70℃時,在剪切模式中,在1赫茲之振盪頻率下測試聚合物片樣品。隨後藉由在溫標(℃)上之損失因數峰之位置確定Tg。
內層之玻璃轉變溫度亦與內層之硬度相關聯--玻璃轉變溫度越高,內層便越硬。一般而言,具有30℃或更高玻璃轉變溫度之內層將使擋風玻璃強度及扭轉剛性增大。另一方面,軟內層(一般特徵在於具有低於30℃之玻璃轉變溫度之內層)有助於聲音阻尼效應(即,聲學特性)。本發明之多層內層透過使用與較軟芯層層壓在一起之較硬或較剛硬皮層(例如,硬//軟//硬)(其中皮層在高壓釜溫度下具有增大之流動)而組合此兩有利性質(即,強度及隔音)。在各種實施例中,多層內層一般包含具有約30℃至約55℃之玻璃轉變溫度之皮層及具有約0℃至約10℃之玻璃轉變溫度之芯層。例如,以下為一些較佳多層組態:(Tg>25℃)//(Tg<10℃)//(Tg>25℃);
(25℃<Tg<55℃)//(Tg<10℃)//(25℃<Tg<55℃);及(25℃<Tg<55℃)//(Tg>-15℃)//(25℃<Tg<55℃)。
此等組態僅作為示例提供且不意欲以任何方式限制本發明所涵蓋之多層組態之類型。然而,有利地,透過在高壓釜處理溫度下具有增大流動之皮層,多層內層將減少冰花缺陷。
藉由已知之水性或溶劑縮醛化方法,透過使聚乙烯醇(PVOH)與丁醛在酸觸媒存在下反應,然後分離、穩定化及乾燥樹脂來製造PVB樹脂。此等縮醛化方法揭示在,例如,美國專利案第2,282,057及2,282,026號及Vinyl Acetal Polymers,Encyclopedia of Polymer Science & Technology,第3版,第8冊,381-399頁,B.E. Wade(2003)中,該等案及文獻之全文內容以引用之方式併入本文。樹脂可以各種形式自市面購置,例如,自Solutia Inc.購置之Butvar® Resin。
如本文中所使用,殘餘羥基含量(以PVOH計)係指在加工完成後殘留在聚合物鏈上之羥基量。例如,可藉由將聚(乙酸乙烯酯)水解成PVOH,及隨後使PVOH與丁醛反應形成PVB來製造PVB。在水解聚(乙酸乙烯酯)之過程中,乙酸酯側基一般不會全部轉化為羥基。此外,與丁醛之反應一般不會導致羥基全部轉化為縮醛基。因此,在任何最終聚(乙烯醇縮丁醛)中,一般將存在殘餘乙酸酯基(如乙酸乙烯酯基)及殘餘羥基(如乙烯羥基)作為聚合物鏈上之側基。如本文中所使用,殘餘羥基含量係依據ASTM 1396基於重量百分比測量。
在各種實施例中,用於皮層及芯層之聚(乙烯醇縮丁醛)樹脂之殘餘羥基含量不同。用於芯層之樹脂,例如,可包含約9至約18重量百分比(重量%)以PVOH計之殘餘羥基,約9至約16重量%以PVOH計之殘餘羥基,或約9至約14重量%以PVOH計之殘餘羥基。用於皮層之樹脂,例如,可包含約13至約35重量百分比(重量%)以PVOH計之殘餘羥基,約13至約30重量%以PVOH計之殘餘羥基,或約15至約22
重量%以PVOH計之殘餘羥基;及最佳地,就某些實施例而言,約17.25至約22.25重量%以PVOH計之殘餘羥基。用於芯層或用於皮層或用於皮層及芯層之樹脂亦可包含小於20重量%殘餘酯基、小於15重量%、小於13重量%、小於11重量%、小於9重量%、小於7重量%、小於5重量%或小於1重量%以聚乙烯酯(例如,乙酸酯)計之殘餘酯基,其餘物質為縮醛,較佳為丁縮醛,但視情況可包括少量其他縮醛基,例如,2-乙基己醛基(參見,例如,美國專利案第5,137,954號,該案以引用全文之方式併入本文)。
值得注意的是,就給定類型之塑化劑而言,塑化劑在聚合物中之相容性主要取決於聚合物之羥基含量。具有較大殘餘羥基含量之聚合物一般與降低之塑化劑相容性或容量相關聯。相對地,具有較低殘餘羥基含量之聚合物一般將導致增大之塑化劑相容性或容量。一般而言,聚合物之殘餘羥基含量與塑化劑相容性/容量之間之此關聯可經操縱及利用,以容許將適量之塑化劑添加至聚合物樹脂及穩定維持多層內層之間之塑化劑含量之差異。
當藉由尺寸排除層析法,利用低角度雷射光散射測量時,存在於習知單層內層及多層內層中之皮層中之標準PVB樹脂一般具有大於約150,000道爾頓之分子量。如本文中所使用,術語「分子量」意指重量平均分子量。然而,出乎意料地,現已發現可使用低分子量皮層(即,小於約140,000道爾頓)來增大PVB內層中之流動,同時不負面影響內層之其他性質。具體言之,所得內層在較高溫度下之流動經有效增大,尤其係在製造(例如,如下文所述之高壓釜處理)期間PVB黏合至玻璃時之溫度下。因此,擋風玻璃及層壓玻璃中之應力值由於擋風玻璃組裝(例如,除氣)及高壓釜處理期間內層部分填充間隙區域而下降。此外,由較低分子量所導致之增大流動不會影響玻璃轉變溫度或層在常溫下之硬度。本發明之高流動內層具有具小於約
140,000道爾頓、小於約135,000道爾頓、小於約130,000道爾頓、小於約125,000道爾頓、小於約120,000道爾頓、小於約115,000道爾頓、小於約110,000道爾頓、小於140,000道爾頓至大於110,000道爾頓之分子量之皮層,及具一般大於約140,000道爾頓、或大於150,000道爾頓、或大於300,000道爾頓之分子量之芯層。在本發明之另一實施例中,本發明之高流動內層具有具小於約140,000道爾頓、小於約130,000道爾頓、小於約120,000道爾頓、小於約110,000道爾頓之分子量之皮層(及具有具一般大於約140,000道爾頓之分子量之芯層)。此等內層已展示50%或更大之冰花形成速率或嚴重性之下降。然而,出乎意料地,聲音傳輸損失、機械及光學性質並未因皮層之流動增大而受負面影響。
如上文及全文所述,經常將本發明之多層內層併入至多層板中,及最常將其佈置在兩基板(如玻璃或丙烯酸系物)及較佳一對玻璃片之間。此種結構之實例將為:(玻璃)//(多層內層)//(玻璃),其中皮層具有不同於內層組成及特性之低分子量、較高塑化劑負載量、兩或更多種塑化劑之混合物、及/或壓紋表面粗糙度。多層板之此等實例不意欲以任何方式施加限制,因本技藝一般熟練者當清楚瞭解,本發明之內層可具有不同於上文所述之許多結構。
使用本發明內層之玻璃層壓板可藉由已知製程製備。在一實施例中,將該聚合物內層及玻璃組裝及加熱至約25℃至60℃之玻璃溫度,及隨後傳送通過一對軋輥以逐出截留空氣,進而形成組合件。經壓縮之組合件隨後經加熱,例如藉由紅外輻射或在對流烘箱中,至約70℃至120℃之溫度。隨後將經加熱之組合件傳送通過第二對軋輥,接著在約130℃至150℃及約1,000至2,000千帕斯卡(kPa)下高壓釜處理該組合件約30分鐘。亦可使用非高壓釜方法,如揭示在美國專利案5,536,347(該案之全文內容以引用之方式併入本文)中之彼等方法。
此外,除軋輥外,本技藝已知用於內層-玻璃界面除氣並在商業上實施之其他方式包括利用真空來移除空氣之真空袋及真空環方法。
為幫助理解本發明之內層,亦可先理解聚合物內層片之相關性質及特性以及用於測量聚合物內層片之此等性質及特性之公式。如本文中所使用之術語「流動」係測量當將一特定點負載壓力(即,4.5 psi)沿厚度方向施加至樣品表面及當將樣品在10℃/分鐘加熱速率下自40℃加熱至135℃時之變形(根據0.76 mm之標準內層厚度標準化之樣品厚度下降)。換言之,當將負載壓力施加至樣品時,PVB「延展」或向側邊流動及施加該負載之點變薄(或發生一定程度變形),使在彼點處之PVB厚度變小;因此,較高變形(即,較大數值)等同於在測試溫度下之較高流動。流動通常係藉由熱-機械分析裝置以DF135測量。例如,在上述測試下,0.242 mm之流動意指具有0.76 mm厚度之內層將沿厚度方向在施加負載壓力之點處變形0.242 mm。多層內層之標準習知皮層具有小於約0.18 mm之流動。另一方面,本發明之皮層具有大於約0.18 mm、大於約0.19 mm、大於約0.20 mm、大於約0.22 mm、大於約0.23 mm、大於約0.24 mm、0.19至約0.26、及約0.19 mm至約0.37 mm之流動。
聚合物應力鬆弛測量提供量化在高溫(如高壓釜處理溫度)下之流動之另一方式。針對本發明皮層之應力鬆弛測量(其利用動態機械分析儀)係透過在150℃下立即將20%剪應力施加至皮層樣品及維持應力恆定,同時成時間之函數測量應力(例如,應力鬆弛模量(G’(t))來確定。隨後將100秒後測得之應力鬆弛模量用於確定相對高壓釜處理流動(帕斯卡)。應力鬆弛模量越低,則聚合物流動越高,且反之亦然。多層內層之標準習知皮層具有大於約110帕斯卡之應力鬆弛模量。另一方面,本發明之皮層具有小於約100帕斯卡、小於約70帕斯卡、小於約50帕斯卡及小於約25帕斯卡之應力鬆弛模量。
如上所述,稱為冰花之光學缺陷常見於三層式層壓板中。可透過模擬在將大型彎曲間隙及除氣不良之組合視為冰花形成之根本原因之擋風玻璃及其他玻璃中之現實情況來測試在三層式隔音PVB層壓板中之冰花形成。首先,將具有放置在中心之聚對苯二甲酸乙二酯(PET)膜環(具有7.5 cm之內徑;14 cm之外徑;及0.10 mm至0.18 mm之厚度)之30 cm×30 cm三層式內層夾在兩30 cm×30 cm玻璃件之間。隨後預層壓及高壓釜處理該結構。使所得層壓板在室溫下平衡48小時,在習知烘箱(80℃)中焙燒48小時,及隨後讓其冷卻。隨後檢視層壓板以確定在層壓板中之冰花形成率(例如,形成冰花缺陷之層壓板之百分比)及在PET環中具有冰花缺陷之面積之百分比,其實例出示在圖3中。此外,檢視層壓板以確定在整個層壓板(包括PET膜區域之內部及外部)內之冰花形成百分比。
亦可測量層壓板之厚度輪廓以確定玻璃之應力。PET膜環之存在使層壓板中產生間隙,該間隙在高壓釜處理熱及壓力下導致玻璃自玻璃邊緣至膜環周圍向內受壓。此外,玻璃在環區域內部向內彎曲及產生下垂效應,如圖4中之虛曲線所示。在環區域內部之下垂在玻璃中產生高度局部化應力。適宜地,本發明內層容許皮層在高壓釜處理溫度下流動至環區域中,及減小下垂並如圖4中之實曲線所示使玻璃應力最小化。兩層壓板均以2.3 mm透明玻璃製成。
本發明之示例性皮層(稱為「本發明層」及如下表1中之DL 1至9所示)及習知皮層(稱為「習知層」及如下表1中之CL 1至3所示)係透過混合及熔化擠壓100份具有不同組成(例如,分子量及PVOH含量)之聚(乙烯醇縮丁醛)樹脂及各種量之塑化劑(如下表1中所示)及其他常見添加劑(如上所述)來製成。隨後藉由上述方法測量皮層之高壓釜處理流動性質。此外,隨後使用表1中所描述之皮層來
建造如表2及表3所示及如下文更完整描述之各種多層內層。
如表1所證實,本發明層具有相較於習知層顯著改良之流動,如藉由對比本發明內層與習知內層之DF135及應力鬆弛測試之結果所示。此外,表1證實流動隨著分子量減小而增大。例如,本發明層1至3及7及習知層3具有相同PVOH含量、塑化劑負載及玻璃轉變溫度,但不同的分子量;及隨著本發明層之分子量減小,流動增大。此外,本發明層5至7各別具有與習知層1至3相同的PVOH含量、塑化劑含量及玻璃轉變溫度,但本發明層5至7具有低得多的分子量。如可見,透過降低分子量,同時維持PVOH含量、塑化劑含量及Tg相同,可顯著增大本發明層之流動。
表1亦證實,可調節塑化劑負載以不僅影響玻璃轉變溫度而且亦影響流動,藉此獲得在室溫下仍十分堅硬之具有極高流動之層。例如,本發明層5至7具有相同PVOH含量及分子量,但塑化劑負載不同。如可見,隨著塑化劑負載增大,玻璃轉變溫度下降(但層保持「堅硬」,即,Tg高於約30℃)且流動增大。
最後,表1亦證實,可透過降低層之PVOH含量來增大流動。例如,本發明層8具有與習知層3相同的分子量及塑化劑含量,但本發明層8具有較低PVOH含量。結果,本發明層8當對比習知層3時具有顯著增大之流動。
在防止本發明示例性內層(稱為「本發明內層」及如以下表2及表3中之DI 1至16所示)形成缺陷方面之改良可透過與先前技藝中之習知多層內層(稱為「習知內層」及如以下表2及表3中之CI 1至4所示)對比而最為清楚明瞭。如上所述,使用表1中所描述之皮層來建造如表2及表3中所顯示之各種多層內層,使用所得之多層內層來建造層壓板。多層內層具有皮層/芯層/皮層之一般結構,其中兩皮層一般具有相同組成及厚度。內層之厚度一般為0.81 mm及芯層之厚度為0.13 mm。表2中之層壓板係以如上所述在中心具有0.13-mm PET膜環之2.3 mm透明玻璃製成。亦軋輥輥壓該等層壓板以進行除氣。隨機粗糙表面內層之平均表面粗糙度(Rz)為約29微米;壓紋表面內層之平均表面粗糙度(Rz)為約38微米。亦以2.3 mm透明玻璃製造表3中之層壓板。對於使用軋輥進行除氣之樣品而言,PET膜環之厚度亦為0.13 mm,但對於使用真空袋進行除氣之樣品而言為0.18 mm。表面粗糙度(Rz)係如表3中所顯示般變化。加熱後表面(Rz)係指如先前所述在100℃下加熱5分鐘後保留之表面。
如在表2及表3中可見,由於高流動皮層使冰花形成顯著減少。具體言之,在冰花測試(其模擬現實彎曲間隙)期間,在環中心中,藉由在標準流動層壓板(具有習知內層)中之高壓釜處理壓力按壓玻璃,藉此使環內之層壓板總厚度輪廓發生下垂。當使用本發明之高流動內層時,該下垂顯著地減小,導致在使用0.18 mm PET膜環及真空袋除氣時之冰花缺陷形成減少32%至86%及在使用0.13 mm PET膜環及軋輥除氣時減少80%至100%。換言之,流動越高,下垂便越小及藉此減少或消除冰花形成。如先前論述,高流動與下垂減小(即,冰花減少)之間之此關係進一步出示於圖4中。
總言之,具有本文中所描述之高流動皮層之多層內層具有超越
本技藝先前使用之習知多層內層的許多優點。一般而言,相較於本技藝先前使用之多層內層,包含如本文中所描述之高流動皮層之多層內層具有增大之流動,其減少多層板中常見缺陷之形成,但不會如本技藝一般熟練者所預期的因流動增大而折損其他性質。熟習本項技術者當可輕易瞭解其他優點。
雖然已結合某些實施例(包括當前據信為較佳實施例之彼等實施例)之描述揭示本發明,然而本詳細描述意欲為說明性且不應理解為限制本發明之範圍。如本技藝一般技術者所當理解,本發明涵蓋在本文中未作詳細描述之實施例。可對所描述之實施例進行修改及變化而不脫離本發明之精神及範圍。
當進一步理解,針對本發明之任何單一組分提出之範圍、值或特性中之任一者可與針對本發明之任何其他組分提出之任何範圍、值或特性互換使用(若適合),以形成具有針對本文全文所提出之組分中之各者定義之值之實施例。例如,可形成包含塑化劑含量在除針對樹脂分子量所提出之範圍中之任一者以外(若適合)之任何範圍內的聚合物層,以形成屬於本發明之範圍內但會造成陳述累贅之許多置換。
Claims (20)
- 一種聚合物內層,其包括:第一聚合物層,其包含具有小於140,000道爾頓之分子量之塑化聚(乙烯醇縮丁醛);第二聚合物層,其包含具有大於140,000道爾頓之分子量之塑化聚(乙烯醇縮丁醛);第三聚合物層,其包含具有小於140,000道爾頓之分子量之塑化聚(乙烯醇縮丁醛);其中該第二聚合物層係佈置在該第一聚合物層與該第三聚合物層之間,藉此獲得具有兩皮層及一芯層之聚合物內層。
- 如請求項1之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有小於130,000道爾頓之分子量。
- 如請求項1之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有小於120,000道爾頓之分子量。
- 如請求項1之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有小於110,000道爾頓之分子量。
- 如請求項1之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有經DF135測量在約0.19 mm至約0.37 mm範圍內之流動。
- 如請求項1之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有介於約25至約55微米之間之壓紋加熱後表面粗糙度Rz。
- 如請求項5之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有小於約100帕斯卡之應力鬆弛模量G’(t)。
- 如請求項1之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有經DF135測量介於約0.19 mm至約0.26 mm之間之流動。
- 如請求項7之聚合物內層,其中該第一聚合物層及該第三聚合物層中之各者包含約30至約60 phr總塑化劑。
- 一種聚合物內層,其包括:第一聚合物層,其包含選自由聚(乙烯醇縮丁醛)、聚胺基甲酸酯及聚(乙烯-共-乙酸乙烯酯)組成之群之至少一種聚合物;第二聚合物層,其包含選自由聚(乙烯醇縮丁醛)、聚胺基甲酸酯及聚(乙烯-共-乙酸乙烯酯)組成之群之至少一種聚合物;其中該第二聚合物層係與該第一聚合物層接觸;及第三聚合物層,其包含選自由聚(乙烯醇縮丁醛)、聚胺基甲酸酯及聚(乙烯-共-乙酸乙烯酯)組成之群之至少一種聚合物;其中該第三聚合物層係與該第二聚合物層接觸;及其中該第二聚合物層係佈置在該第一聚合物層與該第三聚合物層之間,藉此獲得包含兩皮層及一芯層之聚合物內層;及其中該等皮層中之各者具有經DF135測量為約0.19 mm至約0.37 mm之流動。
- 如請求項10之聚合物內層,其中該第一聚合物層及/或該第二聚合物層及/或該第三聚合物層包含聚(乙烯醇縮丁醛)。
- 如請求項11之聚合物內層,其中該等皮層各具有經DF135測量為0.19至0.26 mm之流動。
- 如請求項10之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有介於約25至約55微米之間之壓紋加熱後表面粗糙度Rz。
- 如請求項12之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有小於約100帕斯卡之應力鬆弛模量G’(t)。
- 如請求項14之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有介於約25至約55微米之間之壓紋加熱後表面粗糙度 Rz。
- 如請求項15之聚合物內層,其中該第二聚合物層包含約9至約18重量百分比以PVOH計之殘餘羥基。
- 一種聚合物內層,其包括:第一聚合物層,其包含塑化聚(乙烯醇縮丁醛);第二聚合物層,其包含塑化聚(乙烯醇縮丁醛),且與該第一聚合物層接觸;及第三聚合物層,其包含塑化聚(乙烯醇縮丁醛),且與該第二聚合物層接觸;其中該第二聚合物層係佈置在該第一聚合物層與該第三聚合物層之間,藉此獲得包含兩皮層及一芯層之聚合物內層;及其中至少一皮層具有小於約100帕斯卡之應力鬆弛模量G’(t)。
- 如請求項17之聚合物內層,其中該第一聚合物層及/或該第三聚合物層具有經DF135測量介於約0.19 mm至約0.26 mm之間之流動。
- 如請求項17之聚合物內層,其中該第一聚合物層及/或該第三聚合物層包含約30至約55 phr塑化劑。
- 如請求項17之聚合物內層,其中該第二聚合物層包含約9至約18重量百分比以PVOH計之殘餘羥基。
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US11254111B2 (en) | 2022-02-22 |
WO2013134602A1 (en) | 2013-09-12 |
TWI634989B (zh) | 2018-09-11 |
JP6600022B2 (ja) | 2019-10-30 |
MX357067B (es) | 2018-06-25 |
KR102031612B1 (ko) | 2019-10-14 |
EP2822766A4 (en) | 2015-11-04 |
KR20140138860A (ko) | 2014-12-04 |
US9833976B2 (en) | 2017-12-05 |
JP2015515396A (ja) | 2015-05-28 |
RU2014140743A (ru) | 2016-04-27 |
ZA201405655B (en) | 2015-11-25 |
JP2018086855A (ja) | 2018-06-07 |
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