TW202332722A - Polymer film and uses of the same - Google Patents
Polymer film and uses of the same Download PDFInfo
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- TW202332722A TW202332722A TW111105145A TW111105145A TW202332722A TW 202332722 A TW202332722 A TW 202332722A TW 111105145 A TW111105145 A TW 111105145A TW 111105145 A TW111105145 A TW 111105145A TW 202332722 A TW202332722 A TW 202332722A
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- 229920006254 polymer film Polymers 0.000 title claims abstract description 148
- 239000005340 laminated glass Substances 0.000 claims abstract description 49
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims description 61
- 229920002554 vinyl polymer Polymers 0.000 claims description 48
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- 239000011521 glass Substances 0.000 claims description 35
- 239000004014 plasticizer Substances 0.000 claims description 20
- -1 poly(vinyl butyral) Polymers 0.000 claims description 15
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 13
- 230000009477 glass transition Effects 0.000 claims description 6
- 238000012360 testing method Methods 0.000 description 34
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- RNVXSRJRDVLSAG-UHFFFAOYSA-N 2-[2-(2-benzoyloxypropoxy)propoxy]propyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OC(C)COC(C)COC(C)COC(=O)C1=CC=CC=C1 RNVXSRJRDVLSAG-UHFFFAOYSA-N 0.000 description 1
- GCDUWJFWXVRGSM-UHFFFAOYSA-N 2-[2-(2-heptanoyloxyethoxy)ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOC(=O)CCCCCC GCDUWJFWXVRGSM-UHFFFAOYSA-N 0.000 description 1
- JEYLQCXBYFQJRO-UHFFFAOYSA-N 2-[2-[2-(2-ethylbutanoyloxy)ethoxy]ethoxy]ethyl 2-ethylbutanoate Chemical compound CCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CC JEYLQCXBYFQJRO-UHFFFAOYSA-N 0.000 description 1
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- GYHPTPQZVBYHLC-UHFFFAOYSA-N 2-[2-[2-[2-(2-ethylhexanoyloxy)ethoxy]ethoxy]ethoxy]ethyl 2-ethylhexanoate Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOCCOC(=O)C(CC)CCCC GYHPTPQZVBYHLC-UHFFFAOYSA-N 0.000 description 1
- XFDQLDNQZFOAFK-UHFFFAOYSA-N 2-benzoyloxyethyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCCOC(=O)C1=CC=CC=C1 XFDQLDNQZFOAFK-UHFFFAOYSA-N 0.000 description 1
- UADWUILHKRXHMM-UHFFFAOYSA-N 2-ethylhexyl benzoate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1 UADWUILHKRXHMM-UHFFFAOYSA-N 0.000 description 1
- 229940106004 2-ethylhexyl benzoate Drugs 0.000 description 1
- GPZYYYGYCRFPBU-UHFFFAOYSA-N 6-Hydroxyflavone Chemical compound C=1C(=O)C2=CC(O)=CC=C2OC=1C1=CC=CC=C1 GPZYYYGYCRFPBU-UHFFFAOYSA-N 0.000 description 1
- HNDYULRADYGBDU-UHFFFAOYSA-N 8-methylnonyl benzoate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1 HNDYULRADYGBDU-UHFFFAOYSA-N 0.000 description 1
- UMVMVEZHMZTUHD-UHFFFAOYSA-N DL-Propylene glycol dibenzoate Chemical compound C=1C=CC=CC=1C(=O)OC(C)COC(=O)C1=CC=CC=C1 UMVMVEZHMZTUHD-UHFFFAOYSA-N 0.000 description 1
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 description 1
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- FANBESOFXBDQSH-UHFFFAOYSA-N Ethyladipic acid Chemical compound CCC(C(O)=O)CCCC(O)=O FANBESOFXBDQSH-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- XKGDWZQXVZSXAO-ADYSOMBNSA-N Ricinoleic Acid methyl ester Chemical compound CCCCCC[C@@H](O)C\C=C/CCCCCCCC(=O)OC XKGDWZQXVZSXAO-ADYSOMBNSA-N 0.000 description 1
- XKGDWZQXVZSXAO-SFHVURJKSA-N Ricinolsaeure-methylester Natural products CCCCCC[C@H](O)CC=CCCCCCCCC(=O)OC XKGDWZQXVZSXAO-SFHVURJKSA-N 0.000 description 1
- 238000006359 acetalization reaction Methods 0.000 description 1
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- 230000001070 adhesive effect Effects 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- UADWUILHKRXHMM-ZDUSSCGKSA-N benzoflex 181 Natural products CCCC[C@H](CC)COC(=O)C1=CC=CC=C1 UADWUILHKRXHMM-ZDUSSCGKSA-N 0.000 description 1
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
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- 239000007822 coupling agent Substances 0.000 description 1
- SZLIWAKTUJFFNX-UHFFFAOYSA-N dihydrocitronellol benzoate Natural products CC(C)CCCC(C)CCOC(=O)C1=CC=CC=C1 SZLIWAKTUJFFNX-UHFFFAOYSA-N 0.000 description 1
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 description 1
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- OJXOOFXUHZAXLO-UHFFFAOYSA-M magnesium;1-bromo-3-methanidylbenzene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C1=CC=CC(Br)=C1 OJXOOFXUHZAXLO-UHFFFAOYSA-M 0.000 description 1
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- 229920001223 polyethylene glycol Polymers 0.000 description 1
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- XKGDWZQXVZSXAO-UHFFFAOYSA-N ricinoleic acid methyl ester Natural products CCCCCCC(O)CC=CCCCCCCCC(=O)OC XKGDWZQXVZSXAO-UHFFFAOYSA-N 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
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- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- PZTAGFCBNDBBFZ-UHFFFAOYSA-N tert-butyl 2-(hydroxymethyl)piperidine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCCCC1CO PZTAGFCBNDBBFZ-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
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- 239000005322 wire mesh glass Substances 0.000 description 1
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- Laminated Bodies (AREA)
- Diaphragms For Electromechanical Transducers (AREA)
- Materials For Medical Uses (AREA)
Abstract
Description
本發明係關於一種聚合物膜,特別是關於一種表面具有特定均方根斜率及均方根高度而適用於真空法來進行預壓合的聚合物膜。本發明亦關於一種由該聚合物膜所製得之夾層玻璃。The present invention relates to a polymer film, in particular to a polymer film whose surface has a specific root mean square slope and root mean square height and is suitable for pre-pressing by vacuum method. The invention also relates to a laminated glass produced from the polymer film.
夾層玻璃係一種將聚合物膜夾在二玻璃片中間,藉由熱壓合之方式,使玻璃片與聚合物膜緊密接合而形成之具有複合式結構的玻璃材料。夾層玻璃因具有較佳的耐衝擊性及隔音性,故被廣泛應用於汽車工業與建築工業。Laminated glass is a glass material with a composite structure in which a polymer film is sandwiched between two glass sheets, and the glass sheets and the polymer film are tightly bonded through thermal compression. Laminated glass is widely used in the automotive and construction industries because of its excellent impact resistance and sound insulation.
由於夾層玻璃的製備過程涉及玻璃片與聚合物膜之間的熱壓合,為了避免空氣殘留於夾層玻璃之玻璃片與聚合物膜之間,通常係預先於聚合物膜表面上押花以形成紋路(即,設計凹凸結構),俾使空氣在預壓合期間可被順利排出,從而避免夾層玻璃中產生氣泡。一般而言,預壓合方式可分為真空法及壓輪法。在真空法中,由於加熱時間較長,若聚合物膜的表面紋路太快或太慢潰散,會出現玻璃片與聚合物膜提早封邊而中間的氣泡未完全排出的情形,或是聚合物膜的表面紋路無法完全消除而導致氣泡未完全排出的情形。上述情形均會導致所製得夾層玻璃透明度不佳或存在氣泡瑕疵。Since the preparation process of laminated glass involves thermal pressing between the glass sheet and the polymer film, in order to avoid air remaining between the glass sheet and the polymer film of the laminated glass, the surface of the polymer film is usually embossed in advance to form a pattern. (That is, designing a concave and convex structure) so that air can be smoothly discharged during pre-pressing, thereby avoiding the generation of bubbles in the laminated glass. Generally speaking, pre-pressing methods can be divided into vacuum method and pressure wheel method. In the vacuum method, due to the long heating time, if the surface texture of the polymer film collapses too quickly or too slowly, the glass sheet and the polymer film will be edge-sealed early and the bubbles in the middle will not be completely discharged, or the polymer will The surface texture of the film cannot be completely eliminated, resulting in incomplete discharge of air bubbles. All the above situations will lead to poor transparency or bubble defects in the laminated glass produced.
本發明人研究發現,上述問題意外地可透過控制聚合物膜表面上之均方根斜率(root mean square gradient,Sdq)以及均方根高度(root mean square height,Sq)而獲得解決。因此,本發明係關於一種具有特定均方根斜率及均方根高度的聚合物膜。本發明聚合物膜在夾層玻璃的真空法預壓合製程中可實現優異的預壓合效果,所製得之夾層玻璃不具有氣泡瑕疵且具優良耐候性(於本文中以「高溫氣泡測試」結果展現)。The inventor found through research that the above problem can unexpectedly be solved by controlling the root mean square gradient (Sdq) and the root mean square height (Sq) on the surface of the polymer film. Accordingly, the present invention is directed to a polymer film having a specific root mean square slope and root mean square height. The polymer film of the present invention can achieve excellent pre-pressing effect in the vacuum pre-pressing process of laminated glass, and the produced laminated glass has no bubble defects and excellent weather resistance (herein referred to as "high temperature bubble test" Results are shown).
具體言之,本發明之一目的在於提供一種聚合物膜,其中該聚合物膜具有第一表面及第二表面,其中第一表面的均方根斜率(Sdq)為1.5至3,以及第一表面的均方根高度(Sq)為8微米至20微米,其中Sdq與Sq之定義係依據ISO 25178-2:2012。Specifically, one object of the present invention is to provide a polymer film, wherein the polymer film has a first surface and a second surface, wherein the root mean square slope (Sdq) of the first surface is 1.5 to 3, and the first surface The root mean square height (Sq) of the surface is 8 microns to 20 microns, where the definitions of Sdq and Sq are based on ISO 25178-2:2012.
於本發明之部分實施態樣中,第二表面的Sdq為1.5至3以及第二表面的Sq為8微米至20微米。In some embodiments of the present invention, Sdq of the second surface is 1.5 to 3 and Sq of the second surface is 8 microns to 20 microns.
於本發明之部分實施態樣中,該聚合物膜之玻璃轉移溫度(glass transition temperature,Tg)為5°C至30°C。In some embodiments of the present invention, the polymer film has a glass transition temperature (Tg) of 5°C to 30°C.
於本發明之部分實施態樣中,聚合物膜包含聚乙烯醇縮醛(polyvinylacetal)。In some embodiments of the present invention, the polymer film includes polyvinylacetal.
於本發明之部分實施態樣中,聚乙烯醇縮醛可選自以下群組:聚(乙烯醇縮甲醛)(poly(vinyl formal))、聚(乙烯醇縮乙醛)、聚(乙烯醇縮丁醛)(poly(vinyl butyral))、聚(乙烯醇縮戊醛)、聚(乙烯醇縮己醛)、及其組合。於本發明之較佳實施態樣中,聚乙烯醇縮醛為聚(乙烯醇縮丁醛)。In some embodiments of the present invention, polyvinyl acetal can be selected from the following groups: poly(vinyl formal), poly(vinyl acetal), poly(vinyl alcohol). poly(vinyl butyral), poly(vinyl valeral), poly(vinyl hexaacetal), and combinations thereof. In a preferred embodiment of the present invention, the polyvinyl acetal is poly(vinyl butyral).
於本發明之部分實施態樣中,聚乙烯醇縮醛之重量平均分子量(Mw)為230,000至280,000。In some embodiments of the present invention, the weight average molecular weight (Mw) of the polyvinyl acetal is 230,000 to 280,000.
於本發明之部分實施態樣中,聚合物膜更包含塑化劑。In some embodiments of the present invention, the polymer film further includes a plasticizer.
於本發明之部分實施態樣中,以100重量份之聚乙烯醇縮醛計,塑化劑的含量為30重量份至50重量份。In some embodiments of the present invention, the content of the plasticizer is 30 to 50 parts by weight based on 100 parts by weight of polyvinyl acetal.
於本發明之部分實施態樣中,聚合物膜係具有0.1毫米至2.5毫米之厚度。In some embodiments of the present invention, the polymer film has a thickness of 0.1 mm to 2.5 mm.
本發明之另一目的在於提供一種夾層玻璃,其包含一第一玻璃片、一第二玻璃片、以及位於該第一玻璃片與第二玻璃片之間之中間膜,該中間膜係由如上所述的聚合物膜所提供。Another object of the present invention is to provide a laminated glass, which includes a first glass sheet, a second glass sheet, and an intermediate film located between the first glass sheet and the second glass sheet. The intermediate film is composed of the above The polymer film provided.
為使本發明之上述目的、技術特徵及優點能更明顯易懂,下文係以部分具體實施態樣進行詳細說明。In order to make the above objects, technical features and advantages of the present invention more obvious and easy to understand, some specific implementation aspects are described in detail below.
以下將具體地描述根據本發明之部分具體實施態樣;惟,本發明尚可以多種不同形式之態樣來實踐,不應將本發明保護範圍限於所述具體實施態樣。Some specific implementations according to the present invention will be described in detail below; however, the present invention can still be practiced in many different forms, and the protection scope of the present invention should not be limited to the specific implementations.
除非另有說明, 於本說明書及申請專利範圍中所使用之「一」、「該」及類似用語應理解為包含單數及複數形式。Unless otherwise stated, the terms "a", "the" and similar terms used in this specification and the patent claims shall be understood to include both the singular and the plural.
除非另有說明,於本說明書及申請專利範圍中所使用之「第一」、「第二」及類似用語僅係用於區隔所描述之元件或成分,本身並無特殊涵義,且並非用於代表先後順序。Unless otherwise stated, the terms “first”, “second” and similar terms used in this specification and the scope of the patent application are only used to distinguish the described elements or components. They have no special meanings and are not used. In the order of representation.
於本說明書及申請專利範圍中,用語「均方根斜率(Sdq)」係依據ISO 25178-2:2012而定義。均方根斜率(Sdq)係指在指定範圍內表面上各點的斜率的均方根值,可用於表示表面的陡峭程度。表面完全平坦時,Sdq為0。Sdq越大則表示表面傾斜越陡峭,例如當表面為均勻的45度斜面時,Sdq為1。In this specification and the scope of the patent application, the term "root mean square slope (Sdq)" is defined in accordance with ISO 25178-2:2012. The root mean square slope (Sdq) refers to the root mean square value of the slope of each point on the surface within a specified range, and can be used to express the steepness of the surface. When the surface is completely flat, Sdq is 0. The larger Sdq is, the steeper the slope of the surface is. For example, when the surface is a uniform 45-degree slope, Sdq is 1.
於本說明書及申請專利範圍中,用語「均方根高度(Sq)」係依據ISO 25178-2:2012而定義。均方根高度(Sq)係指在指定範圍內表面上各點的高度的均方根值,相當於高度的標準差。Sq表示的是紋路的高度的一致性,Sq越小表示紋路的高度相近,一致性高。Sq越大表示紋路的高度差異大,一致性低。In this specification and patent application, the term "root mean square height (Sq)" is defined in accordance with ISO 25178-2:2012. The root mean square height (Sq) refers to the root mean square value of the height of each point on the surface within a specified range, which is equivalent to the standard deviation of the height. Sq represents the high consistency of the texture. The smaller the Sq, the higher the consistency of the texture. The larger the Sq, the greater the height difference of the texture and the lower the consistency.
本發明對照現有技術的功效在於,提供一種具有特定均方根斜率及均方根高度的聚合物膜,以及利用該聚合物膜提供無氣泡瑕疵且無白霧瑕疵的透明度良好的夾層玻璃。本發明聚合物膜特別適合利用真空法來進行預壓合。以下就本發明聚合物膜及其相關應用提供詳細說明。Compared with the prior art, the effect of the present invention is to provide a polymer film with a specific root mean square slope and root mean square height, and to use the polymer film to provide laminated glass with good transparency and no bubble defects and no white fog defects. The polymer film of the present invention is particularly suitable for pre-lamination using a vacuum method. The following provides a detailed description of the polymer membrane of the present invention and its related applications.
1.1. 聚合物膜polymer film
1.1.1.1. 聚合物膜的表面特徵Surface Characteristics of Polymer Films
在夾層玻璃的製備過程中,為了使空氣順利排出而不殘留於聚合物膜與玻璃片之間,聚合物膜的表面需要形成有紋路(即,特定的凹凸結構)以利在預壓合期間進行排氣。在預壓合期間,玻璃與聚合物膜之間的氣體的排出是向四面八方進行的,並非僅在單一方向上進行,亦即,排氣問題是發生在二維空間(即,面)中。對此,本發明人研究發現可透過將聚合物膜表面之均方根斜率(Sdq)及均方根高度(Sq)等參數均控制於特定範圍,來解決使用真空法進行夾層玻璃的預壓合時所面臨的排氣問題,能獲致最佳排氣結果,不生氣泡瑕疵或白霧瑕疵,且所製得之夾層玻璃具優異耐候性(以本文所載之「高溫氣泡測試」展現)。所述Sdq及Sq即係與面粗糙度相關的參數,有關Sdq及Sq參數之相關說明可參照ISO25178-2:2012,其為一用於評估表面形貌的測量規範,其全文併於此,以供參考。During the preparation process of laminated glass, in order to allow air to be discharged smoothly without remaining between the polymer film and the glass sheet, the surface of the polymer film needs to be textured (i.e., a specific concave-convex structure) to facilitate the pre-lamination process. Exhaust. During pre-lamination, the gas between the glass and the polymer film is exhausted in all directions, not just in a single direction. That is, the exhaust problem occurs in a two-dimensional space (ie, surface). In this regard, the inventor found that the problem of preloading laminated glass using the vacuum method can be solved by controlling parameters such as the root mean square slope (Sdq) and the root mean square height (Sq) of the polymer film surface within a specific range. The exhaust problems faced at the right time can achieve the best exhaust results without bubble defects or white fog defects, and the laminated glass produced has excellent weather resistance (shown by the "high temperature bubble test" contained in this article) . The Sdq and Sq are parameters related to surface roughness. For relevant descriptions of Sdq and Sq parameters, please refer to ISO25178-2:2012, which is a measurement specification used to evaluate surface topography. Its full text is hereby included. For reference.
具體言之,本發明的聚合物膜具有第一表面及第二表面,其中第一表面的Sdq為1.5至3,例如1.5、1.51、1.52、1.53、1.54、1.55、1.56、1.57、1.58、1.59、1.6、1.61、1.62、1.63、1.64、1.65、1.66、1.67、1.68、1.69、1.7、1.71、1.72、1.73、1.74、1.75、1.76、1.77、1.78、1.79、1.8、1.81、1.82、1.83、1.84、1.85、1.86、1.87、1.88、1.89、1.9、1.91、1.92、1.93、1.94、1.95、1.96、1.97、1.98、1.99、2、2.01、2.02、2.03、2.04、2.05、2.06、2.07、2.08、2.09、2.1、2.11、2.12、2.13、2.14、2.15、2.16、2.17、2.18、2.19、2.2、2.21、2.22、2.23、2.24、2.25、2.26、2.27、2.28、2.29、2.3、2.31、2.32、2.33、2.34、2.35、2.36、2.37、2.38、2.39、2.4、2.41、2.42、2.43、2.44、2.45、2.46、2.47、2.48、2.49、2.5、2.51、2.52、2.53、2.54、2.55、2.56、2.57、2.58、2.59、2.6、2.61、2.62、2.63、2.64、2.65、2.66、2.67、2.68、2.69、2.7、2.71、2.72、2.73、2.74、2.75、2.76、2.77、2.78、2.79、2.8、2.81、2.82、2.83、2.84、2.85、2.86、2.87、2.88、2.89、2.9、2.91、2.92、2.93、2.94、2.95、2.96、2.97、2.98、2.99、或3,或介於由上述任二數值所構成之範圍內。於本發明之較佳實施態樣中,第一表面的Sdq為1.8至2.45。研究顯示,將聚合物膜的第一表面的Sdq值控制在指定範圍內,可在真空法預壓合期間提升排氣效果,避免玻璃片與聚合物膜提早封邊或聚合物膜表面紋路無法被完全消除,預壓合後之夾層玻璃不會發生氣泡瑕疵,且白霧瑕疵亦能被有效抑制。所述「白霧瑕疵」係有少量氣體殘留於聚合物膜中所產生之現象,在白霧瑕疵輕微之情況下,殘留氣體在夾層玻璃正壓合期間可溶入聚合物膜,使得白霧瑕疵消失,此稱為「藏氣」現象。Specifically, the polymer film of the present invention has a first surface and a second surface, wherein the Sdq of the first surface is 1.5 to 3, such as 1.5, 1.51, 1.52, 1.53, 1.54, 1.55, 1.56, 1.57, 1.58, 1.59 ,1.6,1.61,1.62,1.63,1.64,1.65,1.66,1.67,1.68,1.69,1.7,1.71,1.72,1.73,1.74,1.75,1.76,1.77,1.78,1.79,1.8,1.81,1.82,1.83,1.8 4 , 1.85, 1.86, 1.87, 1.88, 1.89, 1.9, 1.91, 1.92, 1.94, 1.95, 1.96, 1.97, 1.98, 2.01, 2.03, 2.07, 2.07, 2.08, 2.08, 2.09 ,2.1,2.11,2.12,2.13,2.14,2.15,2.16,2.17,2.18,2.19,2.2,2.21,2.22,2.23,2.24,2.25,2.26,2.27,2.28,2.29,2.3,2.31,2.32,2.33,2.3 4 . 59 ,2.6,2.61,2.62,2.63,2.64,2.65,2.66,2.67,2.68,2.69,2.7,2.71,2.72,2.73,2.74,2.75,2.76,2.77,2.78,2.79,2.8,2.81,2.82,2.83,2.8 4 , 2.85, 2.86, 2.87, 2.88, 2.89, 2.9, 2.91, 2.92, 2.93, 2.94, 2.95, 2.96, 2.97, 2.98, 2.99, or 3, or within the range composed of any two of the above values. In a preferred embodiment of the present invention, Sdq of the first surface is 1.8 to 2.45. Research shows that controlling the Sdq value of the first surface of the polymer film within a specified range can improve the exhaust effect during vacuum pre-lamination and avoid early edge sealing of the glass sheet and polymer film or failure of the surface texture of the polymer film. are completely eliminated, bubble defects will not occur in the pre-laminated laminated glass, and white fog defects can also be effectively suppressed. The "white fog defect" is a phenomenon caused by a small amount of gas remaining in the polymer film. When the white fog defect is slight, the residual gas can dissolve into the polymer film during the positive lamination of the laminated glass, causing white fog. The defect disappears, which is called "gas storage" phenomenon.
此外,第一表面的Sq為8微米至20微米,例如8微米、8.1微米、8.2微米、8.3微米、8.4微米、8.5微米、8.6微米、8.7微米、8.8微米、8.9微米、9微米、9.1微米、9.2微米、9.3微米、9.4微米、9.5微米、9.6微米、9.7微米、9.8微米、9.9微米、10微米、10.1微米、10.2微米、10.3微米、10.4微米、10.5微米、10.6微米、10.7微米、10.8微米、10.9微米、11微米、11.1微米、11.2微米、11.3微米、11.4微米、11.5微米、11.6微米、11.7微米、11.8微米、11.9微米、12微米、12.1微米、12.2微米、12.3微米、12.4微米、12.5微米、12.6微米、12.7微米、12.8微米、12.9微米、13微米、13.1微米、13.2微米、13.3微米、13.4微米、13.5微米、13.6微米、13.7微米、13.8微米、13.9微米、14微米、14.1微米、14.2微米、14.3微米、14.4微米、14.5微米、14.6微米、14.7微米、14.8微米、14.9微米、15微米、15.1微米、15.2微米、15.3微米、15.4微米、15.5微米、15.6微米、15.7微米、15.8微米、15.9微米、16微米、16.1微米、16.2微米、16.3微米、16.4微米、16.5微米、16.6微米、16.7微米、16.8微米、16.9微米、17微米、17.1微米、17.2微米、17.3微米、17.4微米、17.5微米、17.6微米、17.7微米、17.8微米、17.9微米、18微米、18.1微米、18.2微米、18.3微米、18.4微米、18.5微米、18.6微米、18.7微米、18.8微米、18.9微米、19微米、19.1微米、19.2微米、19.3微米、19.4微米、19.5微米、19.6微米、19.7微米、19.8微米、19.9微米、或20微米,或介於由上述任二數值所構成之範圍內。於本發明之較佳實施態樣中,第一表面的Sq為8.5微米至14.5微米。研究顯示,將聚合物膜的第一表面的Sdq值以及Sq值均控制在指定範圍內,在真空法預壓合期間可獲致最佳之排氣效果,預壓合後之夾層玻璃的白霧瑕疵少,甚至不存在白霧瑕疵,且經過正壓合後之夾層玻璃不存在氣泡瑕疵,同時使得所製得之夾層玻璃具有優異的耐候性(「高溫氣泡測試」結果優異),蓋白霧瑕疵之殘留氣體雖可在夾層玻璃正壓合期間可溶入聚合物膜,但若溶入聚合物膜中的氣體(藏氣)過多,經長時間使用或在較嚴苛條件下,仍會自聚合物膜溶出,形成於夾層玻璃中的氣泡。In addition, Sq of the first surface is 8 microns to 20 microns, such as 8 microns, 8.1 microns, 8.2 microns, 8.3 microns, 8.4 microns, 8.5 microns, 8.6 microns, 8.7 microns, 8.8 microns, 8.9 microns, 9 microns, 9.1 microns , 9.2 micron, 9.3 micron, 9.4 micron, 9.5 micron, 9.6 micron, 9.7 micron, 9.8 micron, 9.9 micron, 10 micron, 10.1 micron, 10.2 micron, 10.3 micron, 10.4 micron, 10.5 micron, 10.6 micron, 10.7 micron, 10.8 Micron, 10.9 micron, 11 micron, 11.1 micron, 11.2 micron, 11.3 micron, 11.4 micron, 11.5 micron, 11.6 micron, 11.7 micron, 11.8 micron, 11.9 micron, 12 micron, 12.1 micron, 12.2 micron, 12.3 micron, 12.4 micron, 12.5 micron, 12.6 micron, 12.7 micron, 12.8 micron, 12.9 micron, 13 micron, 13.1 micron, 13.2 micron, 13.3 micron, 13.4 micron, 13.5 micron, 13.6 micron, 13.7 micron, 13.8 micron, 13.9 micron, 14 micron, 14.1 micron , 14.2 micron, 14.3 micron, 14.4 micron, 14.5 micron, 14.6 micron, 14.7 micron, 14.8 micron, 14.9 micron, 15 micron, 15.1 micron, 15.2 micron, 15.3 micron, 15.4 micron, 15.5 micron, 15.6 micron, 15.7 micron, 15.8 Micron, 15.9 micron, 16 micron, 16.1 micron, 16.2 micron, 16.3 micron, 16.4 micron, 16.5 micron, 16.6 micron, 16.7 micron, 16.8 micron, 16.9 micron, 17 micron, 17.1 micron, 17.2 micron, 17.3 micron, 17.4 micron, 17.5 micron, 17.6 micron, 17.7 micron, 17.8 micron, 17.9 micron, 18 micron, 18.1 micron, 18.2 micron, 18.3 micron, 18.4 micron, 18.5 micron, 18.6 micron, 18.7 micron, 18.8 micron, 18.9 micron, 19 micron, 19.1 micron , 19.2 microns, 19.3 microns, 19.4 microns, 19.5 microns, 19.6 microns, 19.7 microns, 19.8 microns, 19.9 microns, or 20 microns, or within the range composed of any two of the above values. In a preferred embodiment of the present invention, Sq of the first surface is 8.5 microns to 14.5 microns. Research shows that controlling the Sdq value and Sq value of the first surface of the polymer film within the specified range can achieve the best exhaust effect during vacuum pre-lamination. The white mist of the laminated glass after pre-lamination There are few defects, even no white fog defects, and there are no bubble defects in the laminated glass after positive lamination. At the same time, the produced laminated glass has excellent weather resistance (the "high temperature bubble test" result is excellent), covering the white fog. Although the residual gas from defects can be dissolved into the polymer film during the positive lamination process of the laminated glass, if there is too much gas (trapped gas) dissolved into the polymer film, it will still cause damage after long-term use or under harsh conditions. Bubbles formed in laminated glass due to dissolution of the polymer film.
於本發明之較佳實施態樣中,聚合物膜的第二表面亦具有上述Sdq與Sq特徵,亦即第二表面的Sdq為1.5至3,且Sq為8微米至20微米。有關第二表面之Sdq與Sq的具體數值例示可參照第一表面的相關敘述,於此不再贅述。In a preferred embodiment of the present invention, the second surface of the polymer film also has the above-mentioned Sdq and Sq characteristics, that is, the Sdq of the second surface is 1.5 to 3, and the Sq is 8 microns to 20 microns. For specific numerical examples of Sdq and Sq on the second surface, please refer to the relevant description of the first surface, and will not be described again here.
1.2.1.2. 聚合物膜的構成The composition of polymer films
本發明聚合物膜包含聚乙烯醇縮醛作為必要成分,且視需要可進一步包含其他選用成分,如塑化劑或其他習知添加劑。於本發明之部分實施態樣中,聚合物膜係包含聚乙烯醇縮醛及塑化劑,或者聚合物膜實質上係由聚乙烯醇縮醛及塑化劑所構成,或者聚合物膜係由聚乙烯醇縮醛及塑化劑所構成。The polymer film of the present invention contains polyvinyl acetal as an essential component, and may further contain other optional components, such as plasticizers or other conventional additives, if necessary. In some embodiments of the present invention, the polymer film contains polyvinyl acetal and a plasticizer, or the polymer film is essentially composed of polyvinyl acetal and a plasticizer, or the polymer film is Composed of polyvinyl acetal and plasticizer.
本發明聚合物膜可為由單一層構成之單層膜,或由多個層所構成之多層膜,只要聚合物膜整體而言符合所指定之Sdq與Sq之條件即可。於聚合物膜為多層膜之態樣中,聚合物膜各層的材質可為相同或不同,而各自扮演相同或不同之功能層,所述功能層例如是可提供以下一或多種功能之層:隔音功能、隔熱功能、反射功能、抗反射功能、折射功能、抗折射功能、分光功能、及減光功能。The polymer film of the present invention can be a single-layer film composed of a single layer, or a multi-layer film composed of multiple layers, as long as the polymer film as a whole meets the specified conditions of Sdq and Sq. In the case where the polymer film is a multi-layer film, the materials of each layer of the polymer film can be the same or different, and each can play the same or different functional layer. The functional layer can be, for example, a layer that can provide one or more of the following functions: Sound insulation function, heat insulation function, reflection function, anti-reflection function, refraction function, anti-refraction function, light splitting function, and light reduction function.
1.2.1.1.2.1. 聚乙烯醇縮醛polyvinyl acetal
聚乙烯醇縮醛的實例包括但不限於聚(乙烯醇縮甲醛)、聚(乙烯醇縮乙醛)、聚(乙烯醇縮丁醛)、聚(乙烯醇縮戊醛)、及聚(乙烯醇縮己醛)。前述各聚乙烯醇縮醛可單獨使用,亦可混合多種使用。於本發明之較佳實施態樣中,聚乙烯醇縮醛為聚(乙烯醇縮丁醛)。於後附實施例中,聚合物膜係由聚(乙烯醇縮丁醛)與塑化劑所構成。Examples of polyvinyl acetals include, but are not limited to, poly(vinyl formal), poly(vinyl acetal), poly(vinyl butyral), poly(vinyl valeral), and poly(ethylene hexaacetal). Each of the aforementioned polyvinyl acetals can be used individually or in combination. In a preferred embodiment of the present invention, the polyvinyl acetal is poly(vinyl butyral). In the following examples, the polymer film is composed of poly(vinyl butyral) and plasticizer.
聚乙烯醇縮醛的分子量並無特殊限制。於本發明之部分實施態樣中,聚乙烯醇縮醛的重量平均分子量(Mw)可為230,000至280,000,例如230,000、230,500、231,000、231,500、232,000、232,500、233,000、233,500、234,000、234,500、235,000、235,500、236,000、236,500、237,000、237,500、238,000、238,500、239,000、239,500、240,000、240,500、241,000、241,500、242,000、242,500、243,000、243,500、244,000、244,500、245,000、245,500、246,000、246,500、247,000、247,500、248,000、248,500、249,000、249,500、250,000、250,500、251,000、251,500、252,000、252,500、253,000、253,500、254,000、254,500、255,000、255,500、256,000、256,500、257,000、257,500、258,000、258,500、259,000、259,500、260,000、260,500、261,000、261,500、262,000、262,500、263,000、263,500、264,000、264,500、265,000、265,500、266,000、266,500、267,000、267,500、268,000、268,500、269,000、269,500、270,000、270,500、271,000、271,500、272,000、272,500、273,000、273,500、274,000、274,500、275,000、275,500、276,000、276,500、277,000、277,500、278,000、278,500、279,000、279,500、或280,000,或介於由上述任二數值所構成之範圍內,但本發明不以此為限。於本發明之較佳實施態樣中,聚乙烯醇縮醛的Mw為240,000至260,000。The molecular weight of polyvinyl acetal is not particularly limited. In some embodiments of the present invention, the weight average molecular weight (Mw) of the polyvinyl acetal may be 230,000 to 280,000, such as 230,000, 230,500, 231,000, 231,500, 232,000, 232,500, 233,000, 233,500, 234,000, 234,50 0. 235,000 , 235,500, 236,000, 236,500, 237,000, 237,500, 238,000, 238,500, 239,000, 239,500, 240,000, 240,500, 241,000, 241,500, 242,000, 242,500, 243,000, 243,500, 244,000, 244,500, 245,000, 245,500, 246,000, 246,500, 247,000, 247,500 , 248,000, 248,500, 249,000, 249,500, 250,000, 250,500, 251,000, 251,500, 252,000, 252,500, 253,000, 253,500, 254,000, 254,500, 255,000, 255,500, 256,000, 256,500, 257,000, 257,500, 258,000, 258,500, 259,000, 259,500, 260,000 , 260,500, 261,000, 261,500, 262,000, 262,500, 263,000, 263,500, 264,000, 264,500, 265,000, 265,500, 266,000, 266,500, 267,000, 267,500, 268,000, 268,500, 269,000, 269,500, 270,000, 270,500, 271,000, 271,500, 272,000, 272,500 , 273,000, 273,500, 274,000, 274,500, 275,000, 275,500, 276,000, 276,500, 277,000, 277,500, 278,000, 278,500, 279,000, 279,500, or 280,000 , or within the range composed of any two of the above numerical values, but the present invention does not This is the limit. In a preferred embodiment of the present invention, the Mw of polyvinyl acetal is 240,000 to 260,000.
於本發明之部分實施態樣中,以聚乙烯醇縮醛之羥基、縮醛基、乙醯基的總莫耳數計,聚乙烯醇縮醛可具有69莫耳%至75莫耳%的縮醛基含量(即,縮醛度),例如69莫耳%、69.1莫耳%、69.2莫耳%、69.3莫耳%、69.4莫耳%、69.5莫耳%、69.6莫耳%、69.7莫耳%、69.8莫耳%、69.9莫耳%、70莫耳%、70.1莫耳%、70.2莫耳%、70.3莫耳%、70.4莫耳%、70.5莫耳%、70.6莫耳%、70.7莫耳%、70.8莫耳%、70.9莫耳%、71莫耳%、71.1莫耳%、71.2莫耳%、71.3莫耳%、71.4莫耳%、71.5莫耳%、71.6莫耳%、71.7莫耳%、71.8莫耳%、71.9莫耳%、72莫耳%、72.1莫耳%、72.2莫耳%、72.3莫耳%、72.4莫耳%、72.5莫耳%、72.6莫耳%、72.7莫耳%、72.8莫耳%、72.9莫耳%、73莫耳%、73.1莫耳%、73.2莫耳%、73.3莫耳%、73.4莫耳%、73.5莫耳%、73.6莫耳%、73.7莫耳%、73.8莫耳%、73.9莫耳%、74莫耳%、74.1莫耳%、74.2莫耳%、74.3莫耳%、74.4莫耳%、74.5莫耳%、74.6莫耳%、74.7莫耳%、74.8莫耳%、74.9莫耳%、或75莫耳%,或介於由上述任二數值所構成之範圍內。於本發明之較佳實施態樣中,以聚乙烯醇縮醛之羥基、縮醛基、乙醯基的總莫耳數計,聚乙烯醇縮醛可具有71.4莫耳%至73莫耳%的縮醛基含量(即,縮醛度)。In some embodiments of the present invention, based on the total molar number of hydroxyl groups, acetal groups, and acetyl groups of the polyvinyl acetal, the polyvinyl acetal may have a mole content of 69 mol% to 75 mol%. Acetal group content (ie, degree of acetal), such as 69 mol%, 69.1 mol%, 69.2 mol%, 69.3 mol%, 69.4 mol%, 69.5 mol%, 69.6 mol%, 69.7 mol% Ear%, 69.8 Mol%, 69.9 Mol%, 70 Mol%, 70.1 Mol%, 70.2 Mol%, 70.3 Mol%, 70.4 Mol%, 70.5 Mol%, 70.6 Mol%, 70.7 Mol% Ear%, 70.8 Mol%, 70.9 Mol%, 71 Mol%, 71.1 Mol%, 71.2 Mol%, 71.3 Mol%, 71.4 Mol%, 71.5 Mol%, 71.6 Mol%, 71.7 Mol% 71.8 mol%, 71.9 mol%, 72 mol%, 72.1 mol%, 72.2 mol%, 72.3 mol%, 72.4 mol%, 72.5 mol%, 72.6 mol%, 72.7 mol% 72.8 mol%, 72.9 mol%, 73 mol%, 73.1 mol%, 73.2 mol%, 73.3 mol%, 73.4 mol%, 73.5 mol%, 73.6 mol%, 73.7 mol% 73.8 mol%, 73.9 mol%, 74 mol%, 74.1 mol%, 74.2 mol%, 74.3 mol%, 74.4 mol%, 74.5 mol%, 74.6 mol%, 74.7 mol% mol%, 74.8 mol%, 74.9 mol%, or 75 mol%, or within the range composed of any two of the above values. In a preferred embodiment of the present invention, based on the total molar number of hydroxyl groups, acetal groups, and acetyl groups of the polyvinyl acetal, the polyvinyl acetal can have 71.4 mol% to 73 mol%. The acetal group content (i.e., degree of acetalization).
於本發明之部分實施態樣中,以聚乙烯醇縮醛之羥基、縮醛基、乙醯基的總莫耳數計,聚乙烯醇縮醛可具有0莫耳%至1.0莫耳%的乙醯基含量(即,乙醯度),例如0莫耳%、0.05莫耳%、0.1莫耳%、0.15莫耳%、0.2莫耳%、0.25莫耳%、0.3莫耳%、0.35莫耳%、0.4莫耳%、0.45莫耳%、0.5莫耳%、0.55莫耳%、0.6莫耳%、0.65莫耳%、0.7莫耳%、0.75莫耳%、0.8莫耳%、0.85莫耳%、0.9莫耳%、0.95莫耳%、或1.0莫耳%,或介於由上述任二數值所構成之範圍內。於本發明之較佳實施態樣中,以聚乙烯醇縮醛之羥基、縮醛基、乙醯基的總莫耳數計,聚乙烯醇縮醛可具有0莫耳%至0.6莫耳%的乙醯基含量(即,乙醯度)。若聚乙烯醇縮醛的乙醯度高於指定範圍,則聚合物膜相對較軟,押花紋路容易過深。In some embodiments of the present invention, based on the total molar number of hydroxyl groups, acetal groups, and acetyl groups of the polyvinyl acetal, the polyvinyl acetal may have a content of 0 mol% to 1.0 mol%. Acetyl content (ie, acetyl degree), such as 0 mol%, 0.05 mol%, 0.1 mol%, 0.15 mol%, 0.2 mol%, 0.25 mol%, 0.3 mol%, 0.35 mol% 0.4 mol%, 0.45 mol%, 0.5 mol%, 0.55 mol%, 0.6 mol%, 0.65 mol%, 0.7 mol%, 0.75 mol%, 0.8 mol%, 0.85 mol% mol%, 0.9 mol%, 0.95 mol%, or 1.0 mol%, or within the range composed of any two of the above values. In a preferred embodiment of the present invention, based on the total molar number of hydroxyl groups, acetal groups, and acetyl groups of the polyvinyl acetal, the polyvinyl acetal may have 0 mol% to 0.6 mol%. The acetyl content (i.e., degree of acetyl). If the acetyl content of the polyvinyl acetal is higher than the specified range, the polymer film will be relatively soft and the embossed pattern will easily be too deep.
於本發明之部分實施態樣中,以聚乙烯醇縮醛之羥基、縮醛基、乙醯基的總莫耳數計,聚乙烯醇縮醛可具有25莫耳%至30莫耳%的羥基含量,例如25莫耳%、25.1莫耳%、25.2莫耳%、25.3莫耳%、25.4莫耳%、25.5莫耳%、25.6莫耳%、25.7莫耳%、25.8莫耳%、25.9莫耳%、26莫耳%、26.1莫耳%、26.2莫耳%、26.3莫耳%、26.4莫耳%、26.5莫耳%、26.6莫耳%、26.7莫耳%、26.8莫耳%、26.9莫耳%、27莫耳%、27.1莫耳%、27.2莫耳%、27.3莫耳%、27.4莫耳%、27.5莫耳%、27.6莫耳%、27.7莫耳%、27.8莫耳%、27.9莫耳%、28莫耳%、28.1莫耳%、28.2莫耳%、28.3莫耳%、28.4莫耳%、28.5莫耳%、28.6莫耳%、28.7莫耳%、28.8莫耳%、28.9莫耳%、29莫耳%、29.1莫耳%、29.2莫耳%、29.3莫耳%、29.4莫耳%、29.5莫耳%、29.6莫耳%、29.7莫耳%、29.8莫耳%、29.9莫耳%、或30莫耳%,或介於由上述任二數值所構成之範圍內。於本發明之較佳實施態樣中,以聚乙烯醇縮醛之羥基、縮醛基、乙醯基的總莫耳數計,聚乙烯醇縮醛可具有27莫耳%至29莫耳%的羥基含量。若聚乙烯醇縮醛的羥基含量高於指定範圍,則聚合物膜相對較硬,不易形成押花紋路。若聚乙烯醇縮醛的羥基含量低於指定範圍,則聚合物膜相對較軟,押花紋路容易過深。In some embodiments of the present invention, based on the total molar number of hydroxyl groups, acetal groups, and acetyl groups of the polyvinyl acetal, the polyvinyl acetal may have a mole content of 25 to 30 mol%. Hydroxyl content, such as 25 mol%, 25.1 mol%, 25.2 mol%, 25.3 mol%, 25.4 mol%, 25.5 mol%, 25.6 mol%, 25.7 mol%, 25.8 mol%, 25.9 Mol%, 26 Mol%, 26.1 Mol%, 26.2 Mol%, 26.3 Mol%, 26.4 Mol%, 26.5 Mol%, 26.6 Mol%, 26.7 Mol%, 26.8 Mol%, 26.9 Mol%, 27 Mol%, 27.1 Mol%, 27.2 Mol%, 27.3 Mol%, 27.4 Mol%, 27.5 Mol%, 27.6 Mol%, 27.7 Mol%, 27.8 Mol%, 27.9 Mol%, 28 Mol%, 28.1 Mol%, 28.2 Mol%, 28.3 Mol%, 28.4 Mol%, 28.5 Mol%, 28.6 Mol%, 28.7 Mol%, 28.8 Mol%, 28.9 Mol%, 29 Mol%, 29.1 Mol%, 29.2 Mol%, 29.3 Mol%, 29.4 Mol%, 29.5 Mol%, 29.6 Mol%, 29.7 Mol%, 29.8 Mol%, 29.9 Mol%, or 30 mol%, or within the range composed of any two of the above values. In a preferred embodiment of the present invention, based on the total molar number of hydroxyl groups, acetal groups, and acetyl groups of the polyvinyl acetal, the polyvinyl acetal can have 27 mol% to 29 mol%. hydroxyl content. If the hydroxyl content of polyvinyl acetal is higher than the specified range, the polymer film will be relatively hard and difficult to form embossed patterns. If the hydroxyl content of polyvinyl acetal is lower than the specified range, the polymer film will be relatively soft and the embossed pattern will easily be too deep.
1.2.2.1.2.2. 塑化劑Plasticizer
本文中,塑化劑係指可改變熱塑性樹脂的可塑性之化學物質,也可被稱為可塑劑。塑化劑的實例包括但不限於多元酸或多元醇之酯,例如三乙二醇雙(2-乙基己酸酯)(triethylene glycol bis(2-ethylhexanoate))、四乙二醇雙(2-乙基己酸酯)、三乙二醇雙(2-乙基丁酸酯)、四乙二醇雙(2-乙基丁酸酯)、三乙二醇二庚酸酯、四乙二醇二庚酸酯、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、己二酸雙[2-(2-丁氧基乙氧基)乙酯]、聚合己二酸酯(polymeric adipate)、二丙二醇二苯甲酸酯、三丙二醇二苯甲酸酯、聚丙二醇二苯甲酸酯、苯甲酸異癸酯、苯甲酸-2-乙基己酯、丙二醇二苯甲酸酯、鄰苯二甲酸二異壬酯、對苯二甲酸二丁氧基乙酯、蓖麻油、蓖麻油酸甲酯、大豆油、環氧化大豆油、及其組合。於後附實施例中,係使用三乙二醇雙(2-乙基己酸酯)作為塑化劑。In this article, plasticizer refers to a chemical substance that can change the plasticity of thermoplastic resin, and may also be called a plasticizer. Examples of plasticizers include, but are not limited to, esters of polybasic acids or polyhydric alcohols, such as triethylene glycol bis(2-ethylhexanoate), tetraethylene glycol bis(2-ethylhexanoate), -Ethylhexanoate), triethylene glycol bis(2-ethylbutyrate), tetraethylene glycol bis(2-ethylbutyrate), triethylene glycol diheptanoate, tetraethylene glycol Alcohol dihexanate, dihexyl adipate, dioctyl adipate, cyclohexylhexyl adipate, diisononyl adipate, heptyl nonyl adipate, dibutyl sebacate , bis[2-(2-butoxyethoxy)ethyl adipate], polymeric adipate, dipropylene glycol dibenzoate, tripropylene glycol dibenzoate, polypropylene glycol Dibenzoate, isodecyl benzoate, 2-ethylhexyl benzoate, propylene glycol dibenzoate, diisononyl phthalate, dibutoxyethyl terephthalate, trigonite Sesame oil, methyl ricinoleate, soybean oil, epoxidized soybean oil, and combinations thereof. In the attached examples, triethylene glycol bis(2-ethylhexanoate) is used as the plasticizer.
塑化劑之用量並無特殊限制,只要可提供所預之塑化效果即可。一般而言,塑化劑的用量可控制在以100重量份之聚乙烯醇縮醛計為30重量份至50重量份,例如30重量份、31重量份、32重量份、33重量份、34重量份、35重量份、36重量份、37重量份、38重量份、39重量份、40重量份、41重量份、42重量份、43重量份、44重量份、45重量份、46重量份、47重量份、48重量份、49重量份、或50重量份,或介於由上述任二數值所構成之範圍內。於本發明之部分實施態樣中,塑化劑的用量為35重量份至45重量份。There is no special limit on the amount of plasticizer, as long as it can provide the desired plasticizing effect. Generally speaking, the amount of plasticizer can be controlled at 30 to 50 parts by weight based on 100 parts by weight of polyvinyl acetal, such as 30 parts by weight, 31 parts by weight, 32 parts by weight, 33 parts by weight, 34 parts by weight. Parts by weight, 35 parts by weight, 36 parts by weight, 37 parts by weight, 38 parts by weight, 39 parts by weight, 40 parts by weight, 41 parts by weight, 42 parts by weight, 43 parts by weight, 44 parts by weight, 45 parts by weight, 46 parts by weight , 47 parts by weight, 48 parts by weight, 49 parts by weight, or 50 parts by weight, or within the range composed of any two of the above values. In some embodiments of the present invention, the amount of plasticizer is 35 to 45 parts by weight.
1.2.3.1.2.3. 其他習知添加Other common knowledge added 劑agent
習知添加劑可包含任何可適應性改良聚合物膜在製造過程中的可加工性,或賦予聚合物膜特定功能的物質。習知添加劑的實例包括但不限於染料、顏料、穩定劑、抗氧化劑、阻燃劑、紅外線吸收劑、紅外線阻擋劑、紫外線吸收劑、紫外線穩定劑、潤滑劑、分散劑、表面活性劑、螯合劑、耦合劑、黏結劑、及黏著力控制劑。前述各添加劑可單獨使用,亦可混合多種使用。例如,聚合物膜可包含染料或顏料以形成有色聚合物膜,或包含紫外線吸收劑或紅外線吸收劑以形成具有抗紫外線功能之聚合物膜或形成具有抗紅外線功能之聚合物膜。Conventional additives may include any substance that is adaptable to improve the processability of the polymer film during the manufacturing process, or to impart specific functions to the polymer film. Examples of conventional additives include, but are not limited to, dyes, pigments, stabilizers, antioxidants, flame retardants, infrared absorbers, infrared blockers, ultraviolet absorbers, ultraviolet stabilizers, lubricants, dispersants, surfactants, chelates Mixtures, coupling agents, adhesives, and adhesion control agents. Each of the aforementioned additives can be used alone or in combination. For example, the polymer film may include a dye or a pigment to form a colored polymer film, or an ultraviolet absorber or an infrared absorber to form a polymer film with anti-ultraviolet function or a polymer film with anti-infrared function.
1.3.1.3. 聚合物膜的其他性質Other properties of polymer films
1.3.1.1.3.1. 玻璃轉移溫度(Glass transition temperature ( TgTg ))
於本發明之部分實施態樣中,聚合物膜的玻璃轉移溫度(Tg)可控制在5°C至30°C,例如5°C、5.5°C、6°C、6.5°C、7°C、7.5°C、8°C、8.5°C、9°C、9.5°C、10°C、10.5°C、11°C、11.5°C、12°C、12.5°C、13°C、13.5°C、14°C、14.5°C、15°C、15.5°C、16°C、16.5°C、17°C、17.5°C、18°C、18.5°C、19°C、19.5°C、20°C、20.5°C、21°C、21.5°C、22°C、22.5°C、23°C、23.5°C、24°C、24.5°C、25°C、25.5°C、26°C、26.5°C、27°C、27.5°C、28°C、28.5°C、29°C、29.5°C、或30°C,或介於由上述任二數值所構成之範圍內。若聚合物膜的Tg高於指定範圍,則聚合物膜相對較硬,實施機械押花時可能不易形成所欲紋路。若聚合物膜的Tg低於指定範圍,則聚合物膜相對較軟,實施機械押花時所形成的押花紋路過深。於本發明之較佳實施態樣中,聚合物膜的Tg為10°C至25°C。In some embodiments of the present invention, the glass transition temperature (Tg) of the polymer film can be controlled between 5°C and 30°C, such as 5°C, 5.5°C, 6°C, 6.5°C, 7°C. C, 7.5°C, 8°C, 8.5°C, 9°C, 9.5°C, 10°C, 10.5°C, 11°C, 11.5°C, 12°C, 12.5°C, 13°C, 13.5°C, 14°C, 14.5°C, 15°C, 15.5°C, 16°C, 16.5°C, 17°C, 17.5°C, 18°C, 18.5°C, 19°C, 19.5° C, 20°C, 20.5°C, 21°C, 21.5°C, 22°C, 22.5°C, 23°C, 23.5°C, 24°C, 24.5°C, 25°C, 25.5°C, 26°C, 26.5°C, 27°C, 27.5°C, 28°C, 28.5°C, 29°C, 29.5°C, or 30°C, or within the range consisting of any two of the above values . If the Tg of the polymer film is higher than the specified range, the polymer film is relatively hard and it may be difficult to form the desired pattern during mechanical embossing. If the Tg of the polymer film is lower than the specified range, the polymer film is relatively soft and the embossed pattern formed when mechanical embossing is performed is too deep. In a preferred embodiment of the present invention, the polymer film has a Tg of 10°C to 25°C.
1.3.2.1.3.2. 厚度thickness
在符合所指定之Sdq與Sq之條件下,本發明聚合物膜的厚度可視實際需要調整。一般而言,聚合物膜的厚度可為0.1毫米至2.5毫米,例如0.1毫米、0.15毫米、0.2毫米、0.25毫米、0.3毫米、0.35毫米、0.4毫米、0.45毫米、0.5毫米、0.55毫米、0.6毫米、0.65毫米、0.7毫米、0.75毫米、0.8毫米、0.85毫米、0.9毫米、0.95毫米、1.0毫米、1.05毫米、1.1毫米、1.15毫米、1.2毫米、1.25毫米、1.3毫米、1.35毫米、1.4毫米、1.45毫米、1.5毫米、1.55毫米、1.6毫米、1.65毫米、1.7毫米、1.75毫米、1.8毫米、1.85毫米、1.9毫米、1.95毫米、2.0毫米、2.05毫米、2.1毫米、2.15毫米、2.2毫米、2.25毫米、2.3毫米、2.35毫米、2.4毫米、2.45毫米、或2.5毫米,或介於由上述任二數值所構成之範圍內。於後附實施例中,聚合物膜的厚度為0.76毫米。Under the conditions of meeting the specified Sdq and Sq, the thickness of the polymer film of the present invention can be adjusted according to actual needs. Generally speaking, the thickness of the polymer film can be from 0.1 mm to 2.5 mm, such as 0.1 mm, 0.15 mm, 0.2 mm, 0.25 mm, 0.3 mm, 0.35 mm, 0.4 mm, 0.45 mm, 0.5 mm, 0.55 mm, 0.6 mm , 0.65 mm, 0.7 mm, 0.75 mm, 0.8 mm, 0.85 mm, 0.9 mm, 0.95 mm, 1.0 mm, 1.05 mm, 1.1 mm, 1.15 mm, 1.2 mm, 1.25 mm, 1.3 mm, 1.35 mm, 1.4 mm, 1.45 mm, 1.5 mm, 1.55 mm, 1.6 mm, 1.65 mm, 1.7 mm, 1.75 mm, 1.8 mm, 1.85 mm, 1.9 mm, 1.95 mm, 2.0 mm, 2.05 mm, 2.1 mm, 2.15 mm, 2.2 mm, 2.25 mm, 2.3 mm, 2.35 mm, 2.4 mm, 2.45 mm, or 2.5 mm, or within the range composed of any two of the above values. In the following examples, the thickness of the polymer film is 0.76 mm.
1.4.1.4. 聚合物膜之製備Preparation of polymer films
本發明聚合物膜之製備方式並無特殊限制,例如可將聚乙烯醇縮醛與選用成分(如塑化劑)混合捏揉而得到一聚合物膜組合物,再利用習知薄膜製備方法將聚合物膜組合物成膜,並進行機械押花,以利於聚合物膜表面提供所欲之Sdq及Sq。所述薄膜製備方法的實例包括但不限於壓延法、流延法、擠出拉幅法、直接擠出法、及擠出吹塑法。The preparation method of the polymer film of the present invention is not particularly limited. For example, polyvinyl acetal and selected ingredients (such as plasticizers) can be mixed and kneaded to obtain a polymer film composition, and then conventional film preparation methods can be used to prepare the polymer film composition. The polymer film composition is formed into a film and mechanically embossed to facilitate providing the desired Sdq and Sq on the surface of the polymer film. Examples of the film preparation methods include, but are not limited to, calendering, casting, extrusion tentering, direct extrusion, and extrusion blow molding.
於本發明之部分實施態樣中,係以如下方式製備聚合物膜,但本發明並不以此為限:使用混合機將樹脂態之聚乙烯醇縮醛與塑化劑在150°C至250°C之溫度及100 rpm至250 rpm之轉速下混合,並捏揉5分鐘至30分鐘而得到聚合物膜組合物。待聚合物膜組合物冷卻至室溫後,將聚合物膜組合物置於擠出機中擠出成聚合物膜。可視需要重複上述成膜步驟並調整聚合物膜組合物之組成以提供不同功能之膜,並層合各膜,形成具多層結構之聚合物膜。In some embodiments of the present invention, the polymer film is prepared in the following manner, but the present invention is not limited thereto: using a mixer to mix resinous polyvinyl acetal and plasticizer at 150°C to Mix at a temperature of 250°C and a rotation speed of 100 to 250 rpm, and knead for 5 to 30 minutes to obtain a polymer film composition. After the polymer film composition is cooled to room temperature, the polymer film composition is placed in an extruder and extruded into a polymer film. The above film-forming steps may be repeated as necessary and the composition of the polymer film composition may be adjusted to provide films with different functions, and each film may be laminated to form a polymer film with a multi-layer structure.
聚合物膜後續再透過預熱及機械押花即可提供所欲的Sdq及Sq。機械押花係指利用滾輪在成形後的聚合物膜的表面製造紋路。機械押花的方法包括但不限於押花輪法及壓延輪法,其中押花輪法係較佳的。機械押花的紋路樣式並無特殊限制,例如包括菱形、線形、鋸齒形、正方形、錐形、圓形、近似圓形、及不規則形。前述各紋路樣式係可單獨採用,亦可同時採用多種。The polymer film can then provide the desired Sdq and Sq through preheating and mechanical embossing. Mechanical embossing refers to using rollers to create textures on the surface of the formed polymer film. Mechanical embossing methods include but are not limited to the embossing wheel method and the calendering wheel method, among which the embossing wheel method is better. There are no special restrictions on the texture patterns of mechanical embossing, including rhombus, linear, zigzag, square, cone, circle, approximately circle, and irregular shapes. Each of the aforementioned texture styles can be used individually, or multiple types can be used at the same time.
預熱及機械押花條件依照所使用之聚合物膜的組成不同而適應性調整。一般而言,預熱輪溫度可為10°C至100°C,特定言之為30°C至90°C,更特定言之為65°C至85°C。押花輪溫度可為10°C至150°C,特定言之為80°C至140°C,更特定言之為120°C至135°C。押花輪扭力可為0.1 N·m(牛頓.公尺)至1.6 N·m,特定言之為0.5 N·m至1.4 N·m,更特定言之為0.8 N·m至1.3 N·m。押花輪壓力可為2 kg/cm 2(公斤/平方公分)至50 kg/cm 2,特定言之為10 kg/cm 2至45 kg/cm 2,更特定言之為30 kg/cm 2至40 kg/cm 2。 The preheating and mechanical embossing conditions are adaptively adjusted according to the composition of the polymer film used. Generally speaking, the preheating wheel temperature may be from 10°C to 100°C, specifically from 30°C to 90°C, and more specifically from 65°C to 85°C. The embossed wheel temperature may be 10°C to 150°C, specifically 80°C to 140°C, more specifically 120°C to 135°C. The torque of the embossing wheel can be 0.1 N·m (Newton meters) to 1.6 N·m, specifically 0.5 N·m to 1.4 N·m, more specifically 0.8 N·m to 1.3 N·m. The pressure of the embossing wheel can be 2 kg/cm 2 (kg/square centimeter) to 50 kg/cm 2 , specifically 10 kg/cm 2 to 45 kg/cm 2 , more specifically 30 kg/cm 2 to 40 kg/cm 2 .
針對聚合物膜的Sdq與Sq性質,研究發現可透過預熱輪溫度、押花輪溫度、押花輪壓力與押花輪扭力來調整聚合物膜的Sdq與Sq。預熱輪溫度、押花輪溫度與押花輪扭力越大,聚合物膜的Sdq越大。一般而言,預熱輪溫度與押花輪溫度越高,聚合物膜變得較軟而容易壓出較深的紋路,而押花輪扭力越高,越能破壞聚合物膜表面的紋路的均勻性,因此Sdq越高。另外,預熱輪溫度、押花輪溫度與押花輪壓力越大,聚合物膜的Sq越大。一般而言,押花輪壓力越高,越能破壞聚合物膜表面的各點高度的一致性,因此Sq越高。Regarding the Sdq and Sq properties of the polymer film, the study found that the Sdq and Sq of the polymer film can be adjusted through the preheating wheel temperature, the embossing wheel temperature, the embossing wheel pressure and the embossing wheel torque. The greater the preheating wheel temperature, embossing wheel temperature and embossing wheel torque, the greater the Sdq of the polymer film. Generally speaking, the higher the temperature of the preheating wheel and the embossing wheel, the softer the polymer film becomes and it is easier to emboss deeper lines, while the higher the torque of the embossing wheel, the more it will destroy the uniformity of the lines on the surface of the polymer film. , so the higher Sdq. In addition, the greater the preheating wheel temperature, the pattern wheel temperature and the pattern wheel pressure, the greater the Sq of the polymer film. Generally speaking, the higher the pressure of the embossing wheel, the more it can destroy the consistency of the height of each point on the surface of the polymer film, so the higher the Sq.
2.2. 夾層玻璃Laminated glass
本發明之聚合物膜可用於製備夾層玻璃。因此,本發明亦提供一種夾層玻璃,其包含第一玻璃片、第二玻璃片、以及位於該第一玻璃片與第二玻璃片之間之中間膜,該中間膜係由如上所述之聚合物膜所提供。The polymer film of the present invention can be used to prepare laminated glass. Therefore, the present invention also provides a laminated glass, which includes a first glass sheet, a second glass sheet, and an intermediate film located between the first glass sheet and the second glass sheet. The intermediate film is made of the polymer as described above. Provided by the film.
第一玻璃片與第二玻璃片可相同或不同,且可為任何習用於製備夾層玻璃的玻璃片,例如浮法玻璃(float glass)、強化玻璃、夾絲玻璃、或普通平板玻璃,但本發明並不限於此。於後附實施例中,係使用浮法玻璃作為第一玻璃片與第二玻璃片。The first glass sheet and the second glass sheet may be the same or different, and may be any glass sheet conventionally used to prepare laminated glass, such as float glass, tempered glass, wired glass, or ordinary flat glass, but this invention The invention is not limited to this. In the following embodiments, float glass is used as the first glass sheet and the second glass sheet.
本發明之夾層玻璃可藉由相關技術領域中習知的夾層玻璃製備方法而製得。舉例言之,可以如下方式進行夾層玻璃之製備:將聚合物膜夾置於二玻璃片之間以得到一積層物,將積層物放入真空袋中並在20°C至30°C的溫度下抽真空(真空度>500 mmHg(毫米汞柱),例如600 mmHg至700 mmHg)至少10分鐘,接著將裝有積層物之真空袋放入加熱爐中,從60°C緩慢升溫至150°C,至少歷時15分鐘之後,將真空袋從加熱爐中取出,完成預壓合。所得到的預壓合後的積層物的玻璃片的表面溫度為90°C至110°C。接著將預壓合後之積層物置於高壓釜中進行正壓合,於高溫高壓條件下熱壓100分鐘至150分鐘,製得夾層玻璃。一般而言,所述高溫高壓條件可為10巴至15巴的壓力及100°C至150°C的溫度。The laminated glass of the present invention can be produced by conventional laminated glass preparation methods in the relevant technical fields. For example, laminated glass can be prepared as follows: a polymer film is sandwiched between two glass sheets to obtain a laminate, which is placed in a vacuum bag and heated at a temperature of 20°C to 30°C. Apply vacuum (vacuum degree >500 mmHg (millimeters of mercury), such as 600 mmHg to 700 mmHg) for at least 10 minutes, then place the vacuum bag containing the laminate into the heating furnace and slowly increase the temperature from 60°C to 150°C. C. After at least 15 minutes, take the vacuum bag out of the heating furnace and complete the pre-pressing. The surface temperature of the glass sheet of the obtained prelaminated laminate was 90°C to 110°C. Then, the pre-pressed laminate is placed in an autoclave for forward pressing, and hot-pressed under high temperature and high pressure conditions for 100 to 150 minutes to prepare laminated glass. Generally speaking, the high temperature and high pressure conditions may be a pressure of 10 bar to 15 bar and a temperature of 100°C to 150°C.
3.3. 實施例Example
3.1.3.1. 測量方式說明Measurement method description
茲以下列具體實施態樣進一步例示說明本發明,其中,所採用之測量儀器及方法分別如下:The present invention is further illustrated by the following specific embodiments, in which the measuring instruments and methods used are as follows:
[聚乙烯醇縮醛之分子量的測量][Measurement of molecular weight of polyvinyl acetal]
利用膠體滲透層析法( gel permeation chromatography ,GPC)來測量聚乙烯醇縮醛之分子量分布,其中係將聚乙烯醇縮醛溶解於四氫呋喃(tetrahydrofuran,THF)中,在以下條件下進行GPC分析,並以對應聚苯乙烯標準品(Waters PS STD)面積的比率計算其分子量。 裝置:Waters 1515 PUMP system 探測器:Waters 2414 RI 沖提條件:1.0毫升/分鐘(mL/min),THF 管柱:Waters Styragel HR5 THF、Waters Styragel HR4 THF、Waters Styragel HR3 THF、Waters Styragel HR1 THF The molecular weight distribution of polyvinyl acetal is measured using gel permeation chromatography (GPC). The polyvinyl acetal is dissolved in tetrahydrofuran (THF), and GPC analysis is performed under the following conditions. And calculate its molecular weight based on the ratio of the area of the corresponding polystyrene standard (Waters PS STD). Device: Waters 1515 PUMP system Detector: Waters 2414 RI Extraction conditions: 1.0 ml/min (mL/min), THF Column: Waters Styragel HR5 THF, Waters Styragel HR4 THF, Waters Styragel HR3 THF, Waters Styragel HR1 THF
[聚乙烯醇縮醛之縮醛度、乙醯度及羥基含量的測量][Measurement of acetal degree, acetyl degree and hydroxyl content of polyvinyl acetal]
聚乙烯醇縮醛的縮醛度、乙醯度及羥基含量係依據JIS K6728所測得。The acetal degree, acetyl degree and hydroxyl content of polyvinyl acetal are measured according to JIS K6728.
[玻璃轉移溫度(Tg)的測量][Measurement of glass transition temperature (Tg)]
利用差示掃描量熱儀(型號:TA DSC 25,購自TA儀器(TA Instruments))在氮氣氛圍下測量聚合物膜的Tg。首先,取7毫克的聚合物膜作為樣品放入差示掃描量熱儀的樣品載台上,以10°C/分鐘之升溫速率升溫至150°C後在該溫度下保持5分鐘。接著,使樣品在-50°C平衡並在該溫度下保持5分鐘,接著,以10°C/分鐘之升溫速率升溫至100°C而得到溫度對熱流(heat flow)的曲線圖(X軸為溫度,Y軸為熱流),並將玻璃轉化中點(midpoint)所對應的溫度記錄為Tg。The Tg of the polymer film was measured using a differential scanning calorimeter (model: TA DSC 25, purchased from TA Instruments) under nitrogen atmosphere. First, take 7 mg of polymer film as a sample and place it on the sample stage of the differential scanning calorimeter. The temperature is raised to 150°C at a heating rate of 10°C/min and then maintained at this temperature for 5 minutes. Next, the sample was equilibrated at -50°C and maintained at this temperature for 5 minutes. Then, the temperature was increased to 100°C at a heating rate of 10°C/min to obtain a curve of temperature versus heat flow (X-axis). is the temperature, the Y-axis is the heat flow), and the temperature corresponding to the glass transition midpoint (midpoint) is recorded as Tg.
[Sdq及Sq的測量][Measurement of Sdq and Sq]
首先, 於聚合物膜的幅寬方向上分別選取兩端及中間共三個部分,裁切成三個3公分×3公分的測試樣品。在24±3°C之溫度與63±3%之相對溼度下,根據ISO 25178-2:2012之規範,利用雷射掃描共軛焦顯微鏡(laser scanning confocal microscope)(型號:LEXT OLS5000-SAF,購自奧林巴斯(Olympus))來分析聚合物膜的表面紋路,可得到聚合物膜的Sdq及Sq。將三個測試樣品的Sdq及Sq進行平均,得到各聚合物膜的Sdq及Sq。詳細分析條件如下:光源具有450奈米之波長,接物鏡倍率為100倍(MPLAPON-100xLEXT),光學變焦(optical zoom)為50倍,圖像面積為1500微米×1500微米,解析度為1024像素×1024像素,操作條件設定為自動傾斜去除(auto tilt removal),以及不使用濾光片。Sq的單位為微米。First, select three parts at both ends and the middle in the width direction of the polymer film, and cut them into three test samples of 3 cm x 3 cm. At a temperature of 24±3°C and a relative humidity of 63±3%, a laser scanning conjugate microscope (model: LEXT OLS5000-SAF) was used in accordance with the specifications of ISO 25178-2:2012. (purchased from Olympus) to analyze the surface texture of the polymer film, and the Sdq and Sq of the polymer film can be obtained. The Sdq and Sq of the three test samples were averaged to obtain the Sdq and Sq of each polymer film. The detailed analysis conditions are as follows: the light source has a wavelength of 450 nanometers, the objective lens magnification is 100 times (MPLAPON-100xLEXT), the optical zoom (optical zoom) is 50 times, the image area is 1500 microns × 1500 microns, and the resolution is 1024 pixels ×1024 pixels, operating conditions set to auto tilt removal, and no filter used. The unit of Sq is micrometer.
[預壓合測試][Pre-pressure test]
首先,將聚合物膜夾置於二片潔淨的透明浮法玻璃片(長度為300毫米、寬度為300毫米、厚度為2毫米)之間以得到一積層物。接著,將積層物放入烘箱中,在以下條件下進行預壓合測試:持續抽真空以維持在700 mmHg的真空度下進行三段持溫測試,第一段持溫溫度為30°C且持溫時間為10分鐘,第二段持溫溫度為140°C且持溫時間為40分鐘,第三段持溫溫度為40°C且持溫時間為30分鐘。之後,以肉眼觀察積層物是否有白霧出現,並依以下標準評估。
預壓合測試之實益在於,若白霧出現區域面積太大(例如大於玻璃總面積的20%),表示聚合物膜的表面有大量的空氣殘留,則之後在高壓釜中進行夾層玻璃的正壓合時,表面殘留的空氣將無法被聚合物膜完全吸收,導致夾層玻璃中出現氣泡瑕疵。The practical benefit of the pre-lamination test is that if the area where the white fog appears is too large (for example, greater than 20% of the total area of the glass), it means that there is a large amount of air remaining on the surface of the polymer film, and then the laminated glass will be normalized in an autoclave. During lamination, the air remaining on the surface will not be completely absorbed by the polymer film, resulting in bubble defects in the laminated glass.
[高溫氣泡測試(耐候性評估)][High temperature bubble test (weather resistance evaluation)]
將夾層玻璃裁切成30公分×30公分的測試樣品。將測試樣品以垂直置放之方式放入100°C的烘箱中歷時2小時之後,取出並以肉眼觀察測試樣品是否有氣泡出現,且依以下標準來評估。
高溫氣泡測試的實益在於,即使夾層玻璃在製備完成時呈現無氣泡瑕疵之狀態,若聚合物膜中有過多溶入之氣體(藏氣),則在夾層玻璃歷經高溫測試後,氣體會溶出形成氣泡,此即,這類夾層玻璃耐候性不佳,不利於長期使用。The practical benefit of the high-temperature bubble test is that even if the laminated glass appears to be bubble-free when the preparation is completed, if there is too much dissolved gas (trapped gas) in the polymer film, the gas will dissolve and form after the laminated glass undergoes the high-temperature test. Bubbles, that is, this type of laminated glass has poor weather resistance and is not conducive to long-term use.
3.2.3.2. 聚合物膜的製備及性質測量Preparation and property measurement of polymer films
首先,將100重量份的聚(乙烯醇縮丁醛)(PVB,購自長春石油化學股份有限公司)與40重量份的塑化劑(三乙二醇雙(2-乙基己酸酯))混合而得到一混合物,使用混合機在200°C下以150 rpm之旋轉速度捏揉該混合物15分鐘之後,冷卻至室溫而得到一聚合物膜組合物。接著,將聚合物膜組合物置於擠出機中,擠出成厚度為0.76毫米的聚合物膜。依照前文所載方法測量所使用的PVB的Mw、縮醛度、乙醯度與羥基含量比以及所製得的聚合物膜的Tg,結果如下:PVB的Mw為約250,000、PVB的縮醛度為71.6莫耳%、PVB的乙醯度為0.4莫耳%、PVB的羥基含量為28莫耳%、聚合物膜的Tg為約15°C。First, 100 parts by weight of poly(vinyl butyral) (PVB, purchased from Changchun Petrochemical Co., Ltd.) and 40 parts by weight of a plasticizer (triethylene glycol bis(2-ethylhexanoate) ) to obtain a mixture. Use a mixer to knead the mixture at a rotation speed of 150 rpm at 200°C for 15 minutes, and then cool to room temperature to obtain a polymer film composition. Next, the polymer film composition was placed in an extruder and extruded into a polymer film with a thickness of 0.76 mm. According to the method mentioned above, the Mw, acetal degree, acetal degree and hydroxyl content ratio of the PVB used and the Tg of the produced polymer film were measured. The results are as follows: the Mw of PVB is about 250,000 and the acetal degree of PVB. It is 71.6 mol%, the acetyl content of PVB is 0.4 mol%, the hydroxyl content of PVB is 28 mol%, and the Tg of the polymer film is about 15°C.
根據表1-1及表1-2所示參數條件對聚合物膜的二表面進行預熱及機械押花,得到實施例1至6及比較例1至6的聚合物膜。除了表1-1及表1-2所示參數條件之外,聚合物膜通過押花輪之間的線速度為3 m/min。依照前文所載方法測量實施例1至6及比較例1至6的聚合物膜的Sdq及Sq,並將結果記錄於表2-1至表2-2中。The two surfaces of the polymer film were preheated and mechanically embossed according to the parameter conditions shown in Table 1-1 and Table 1-2 to obtain polymer films of Examples 1 to 6 and Comparative Examples 1 to 6. In addition to the parameter conditions shown in Table 1-1 and Table 1-2, the linear speed of the polymer film passing between the embossing wheels is 3 m/min. The Sdq and Sq of the polymer films of Examples 1 to 6 and Comparative Examples 1 to 6 were measured according to the methods described above, and the results were recorded in Tables 2-1 to 2-2.
表1-1:實施例1至6的聚合物膜的機械押花參數條件
表1-2:比較例1至6的聚合物膜的機械押花參數條件
表2-1:實施例1至6的聚合物膜的性質
表2-2:比較例1至6的聚合物膜的性質
3.3.3.3. 夾層玻璃之製備及性質評估Preparation and property evaluation of laminated glass
分別使用實施例1至6及比較例1至6的聚合物膜來製備夾層玻璃。首先,將聚合物膜裁切成300毫米×300毫米的大小。接著,準備二片潔淨的透明浮法玻璃片(長度為300毫米、寬度為300毫米、厚度為2毫米),並將裁切後的聚合物膜夾在二片透明浮法玻璃片之間而得到一積層物,利用真空袋式方法對積層物進行抽真空,以進行預壓合。真空袋式的操作方式係如下所述:將積層物放入真空袋中並在30°C之溫度下以700 mmHg的真空度保持10分鐘,接著將裝有積層物之真空袋放入加熱爐中,在140°C之溫度下維持40分鐘,之後將真空袋從加熱爐中取出並在室溫下冷卻。冷卻後解開真空並取出積層物。將經預壓合之積層物置於高壓釜中以13巴的壓力及135°C的溫度壓合120分鐘,接著冷卻至室溫,製得夾層玻璃。Laminated glass was prepared using the polymer films of Examples 1 to 6 and Comparative Examples 1 to 6 respectively. First, the polymer film is cut into a size of 300 mm x 300 mm. Next, prepare two clean transparent float glass sheets (length 300 mm, width 300 mm, thickness 2 mm), and sandwich the cut polymer film between the two transparent float glass sheets. A laminated product is obtained, and the laminated product is evacuated using a vacuum bag method to perform pre-pressing. The operation method of the vacuum bag type is as follows: put the laminate into the vacuum bag and maintain it at a temperature of 30°C with a vacuum degree of 700 mmHg for 10 minutes, and then put the vacuum bag containing the laminate into the heating furnace in, maintaining the temperature at 140°C for 40 minutes, after which the vacuum bag is taken out of the heating oven and cooled at room temperature. After cooling, release the vacuum and take out the laminate. The pre-pressed laminate was placed in an autoclave and pressed at a pressure of 13 bar and a temperature of 135°C for 120 minutes, and then cooled to room temperature to prepare laminated glass.
依照前文所載方法,對實施例1至6及比較例1至6的聚合物膜以及夾層玻璃進行預壓合測試以及高溫氣泡測試,並將結果紀錄於表3-1及表3-2中。According to the methods described above, pre-pressure tests and high-temperature bubble tests were performed on the polymer films and laminated glasses of Examples 1 to 6 and Comparative Examples 1 to 6, and the results were recorded in Table 3-1 and Table 3-2 .
表3-1:實施例1至6的聚合物膜所製夾層玻璃的評估結果
表3-2:比較例1至6的聚合物膜所製夾層玻璃的評估結果
如表3-1所示,本發明聚合物膜在真空法預壓合測試中可獲得令人滿意的結果且由本發明聚合物膜所製得的夾層玻璃在高溫氣泡測試中亦可獲得令人滿意的結果,顯示夾層玻璃之耐候性佳。實施例1至6顯示,當聚合物膜的Sdq及Sq均在指定範圍內時,可在真空法的預壓合測試中獲得令人滿意的結果且所製得夾層玻璃亦可在高溫氣泡測試中獲得令人滿意的結果。尤其,實施例1、5及6顯示,在Sdq為1.8至2.45時可獲致最優異的預壓合測試結果,且實施例1至2、4至5顯示,在Sq為8.5微米至14.5微米時可獲致最優異的高溫氣泡測試結果。As shown in Table 3-1, the polymer film of the present invention can obtain satisfactory results in the vacuum pre-pressure test, and the laminated glass made from the polymer film of the present invention can also obtain satisfactory results in the high-temperature bubble test. The satisfactory results show that the laminated glass has good weather resistance. Examples 1 to 6 show that when the Sdq and Sq of the polymer film are both within the specified range, satisfactory results can be obtained in the pre-lamination test by the vacuum method and the prepared laminated glass can also be used in the high-temperature bubble test. obtain satisfactory results. In particular, Examples 1, 5 and 6 show that the best pre-laminated test results are obtained when Sdq is 1.8 to 2.45, and Examples 1 to 2, 4 to 5 show that Sq is 8.5 microns to 14.5 microns. Gets the best high-temperature bubble test results.
相較於此,如表3-2所示,不屬於本發明的聚合物膜在真空法預壓合測試中無法獲得令人滿意的結果,且所製得的夾層玻璃在高溫氣泡測試中亦無法獲得令人滿意的結果。比較例2及3顯示,即使聚合物膜的Sq在指定範圍內,只要Sdq不在指定範圍內,聚合物膜在真空法預壓合測試中無法獲得令人滿意的結果,且所製得的夾層玻璃在高溫氣泡測試中亦無法獲得令人滿意的結果。比較例4顯示,即使聚合物膜的Sdq在指定範圍內,只要Sq不在指定範圍內,所製得的夾層玻璃在高溫氣泡測試中無法獲得令人滿意的結果,顯示耐候性不佳。比較例1、5及6顯示,若聚合物膜的Sdq與Sq均不在指定範圍內,則在真空法預壓合測試中無法獲得令人滿意的結果,且所製得的夾層玻璃在高溫氣泡測試中亦無法獲得令人滿意的結果。In comparison, as shown in Table 3-2, the polymer film that does not belong to the present invention cannot obtain satisfactory results in the vacuum pre-pressure test, and the prepared laminated glass also fails in the high-temperature bubble test. Unable to obtain satisfactory results. Comparative Examples 2 and 3 show that even if the Sq of the polymer film is within the specified range, as long as the Sdq is not within the specified range, the polymer film cannot obtain satisfactory results in the vacuum pre-lamination test, and the resulting sandwich Glass also failed to obtain satisfactory results in high-temperature bubble tests. Comparative Example 4 shows that even if the Sdq of the polymer film is within the specified range, as long as the Sq is not within the specified range, the prepared laminated glass cannot obtain satisfactory results in the high-temperature bubble test and shows poor weather resistance. Comparative Examples 1, 5 and 6 show that if the Sdq and Sq of the polymer film are not within the specified range, satisfactory results cannot be obtained in the vacuum pre-pressure test, and the laminated glass produced will bubble at high temperatures. Satisfactory results could not be obtained during testing.
上述實施例僅為例示性說明本發明之原理及其功效,並闡述本發明之技術特徵,而非用於限制本發明之保護範疇。任何熟悉本技術者在不違背本發明之技術原理下,可輕易完成之改變或安排,均屬本發明所主張之範圍。因此,本發明之權利保護範圍係如後附申請專利範圍所列。The above embodiments are only for illustrating the principles and effects of the present invention and elucidating the technical features of the present invention, but are not intended to limit the scope of protection of the present invention. Any changes or arrangements that can be easily made by those familiar with the art without violating the technical principles of the invention fall within the scope of the invention. Therefore, the protection scope of the present invention is as listed in the appended patent application scope.
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