CN106660239B - 用于制备基于增塑聚乙烯醇缩醛的压纹膜的方法 - Google Patents
用于制备基于增塑聚乙烯醇缩醛的压纹膜的方法 Download PDFInfo
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Abstract
本发明涉及一种方法,用于通过以下方法步骤将包含增塑聚乙烯醇缩醛的膜压纹,以使在至少一个表面上的粗糙度Rz为20至100µm:a.将增塑聚乙烯醇缩醛挤出成表面的随机粗糙度Rz=1至70µm的膜,b.将步骤a)中获得的膜的至少一个表面压上具有5‑50µm的深度、10‑200µm的宽度和50‑2500µm的间距的槽,其中c.所述槽之间的隆起的表面粗糙度比步骤a)中所获得的低至多20%。
Description
背景技术
本发明涉及用于通过压纹来制备基于增塑聚乙烯醇缩醛的膜的方法并涉及所述膜用于制备玻璃层压件的用途。
层压的安全玻璃通常由两块玻璃板(glass pane)和一种粘合膜组成,所述粘合膜将所述玻璃板结合在一起并且基于增塑聚乙烯醇缩醛,优选聚乙烯醇缩丁醛(PVB)。层压的安全玻璃特别用作机动车的挡风玻璃,如果需要,玻璃板可能被聚合物板替代。
在建筑业中,硅酸盐玻璃/硅酸盐玻璃复合材料或硅酸盐玻璃/聚合物复合材料也用作例如窗玻璃或用作中间墙,如果需要并且根据其应用,例如作为防弹玻璃,使用多重复合材料,即由超过两个支撑层组成的复合材料。
用于制造安全复合玻璃的基于聚乙烯醇缩醛,特别是基于聚乙烯醇缩丁醛(PVB)的含增塑剂的膜即使在室温下也是软的并发粘。尽管高粘着性对于将复合玻璃中的玻璃/膜/玻璃的复合材料保持在一起是必要的,但对于运输和将它们加工成这种玻璃的过程而言,该粘着性需要被暂时消除,或然而,至少被抑制。膜的固有粘着性可通过一定的粗糙度降低。
此外,在加工所述膜以形成复合安全玻璃期间需要可能除去膜和玻璃之间存在的空气。在这方面,通常已知在膜的一个或两个面上提供粗糙化表面。在玻璃层压件制造期间封入的空气能够经由该粗糙化表面逃逸从而获得无气泡的层压件。
用于制造具有粗糙化表面的膜的典型方法从EP 0 185 863 B1中作为熔体破裂方法已知。熔体破裂方法导致不规则地(随机地)粗糙化表面。
压纹方法是用于产生粗糙化表面的目前工艺水平中描述的其它方法。通过压纹方法产生的所有膜表面的共同特征是规则的(非随机的)表面结构,其展示良好的通风性能(ventilation behaviour),特别在通过真空袋法制备玻璃层压件的过程中,并因此允许短的加工时间和宽的加工窗口。
与熔体破裂方法相比,压纹方法具有获得的规则表面结构允许在层压件制备期间更快速且更简单地去除空气的优点。
EP 0 741 640 B1描述了借助两个压纹辊产生在两个面上压纹的表面的这种压纹方法,借助它提供所述膜以规则的锯齿类型的线结构。在所述膜的各面上压印(emboss)的线以>25°的角度相互交错从而防止在复合玻璃中形成所谓的莫尔纹。
EP 1 233 007 A1公开了用于避免莫尔效应的压纹方法,所述方法在膜的各面上产生规则的压纹结构。为了避免干涉,两个膜面的线结构具有不同的重复频率。
US 5,972,280中描述的另一方法仅使用一个辊(而不是两个压纹辊)和经由滚筒(roll)和压缩空气紧贴配合至该辊的结构化钢带来压印表面结构,在压纹过程期间膜被引导通过压纹辊和钢带之间的间隙。
US 4,671,913公开了将PVB膜压纹的方法,所述膜在单一操作过程中在两个结构化辊之间被压纹。所述辊以及还有因此的压纹膜具有10至60 µm的粗糙度Rz。US 2003/0022015、WO 01/72509、US 6077374和US 60934741 描述了借助钢的压纹辊和具有橡胶涂层的压辊的用于PVB膜的单阶段和两阶段压纹方法。
WO 2014021459 A1公开了通过压印具有至少750 µm的宽间距(pitch)的槽制造增塑PVB膜。
为了有效地制备层压玻璃,中间层应具有良好的除气性质以及表面结构的快速熔化。
发明公开
本发明的目的是一种方法,其用于通过以下方法步骤将包含增塑聚乙烯醇缩醛的膜压纹,以 使在至少一个表面上的粗糙度Rz为20至100μm:
a.将增塑聚乙烯醇缩醛挤出成表面的随机粗糙度Rz=1至70μm的膜,
b.将步骤a)中获得的膜的至少一个表面压上具有5-50μm的深度、10-250μm的宽度,优选 10-200μm的宽度和50-2500μm的间距的槽,其中
c.所述槽之间的隆起(elevation)的表面粗糙度比步骤a)中所获得的低至多20%。
所述槽之间的隆起上的随机表面图案在步骤a)期间产生并且应在压纹步骤b)期间保持与步骤a)期间获得的基本上相同。
优选,步骤b)中获得的槽之间的隆起的表面粗糙度比步骤a)中获得的低至多10%,更优选至多5%。最好地,步骤a)和步骤b)中获得的槽之间的隆起的表面粗糙度(保持)相同。这可通过压纹工具实现,所述压纹工具与隆起区域中的膜不具有接触或不具有完全接触。
步骤a)中包含增塑聚乙烯醇缩醛的熔体的挤出优选在熔体破裂条件下、使用具有唇口(lip)的挤出模头进行,所述唇口的温度可以调节。这种挤出方法对于本领域技术人员而言是已知的,例如来自EP 0 185 863 B1。
在所述膜的表面上,槽之间的隆起上的随机表面图案可相同或不同。可通过在熔体破裂挤出期间改变排出间隙(discharge gap)的宽度和正好在模头出口上的模唇的温度来产生不同的表面图案或粗糙度水平。
优选进行步骤a)以获得表面的随机粗糙度Rz = 10至70 µm的膜,且更优选获得表面的随机粗糙度Rz = 30至70 µm的膜。
在本发明的第一变体中,所述挤出在熔体破裂条件下进行,其中挤出模头具有100-270℃,优选100-240℃的唇口温度。
在本发明的第二变体中,在熔体破裂条件下的挤出以500-3500 kg/h的熔体流动速率进行。
在挤出之后,所述膜在步骤b)中在一个或两个面上经受压纹,以使在各种情况下独立地具有Rz =20至100 µm,优选Rz = 20至80 µm,特别地Rz = 25 µm至70 µm的表面结构和粗糙度深度。
步骤a)中获得的膜的表面可在单一步骤中或优选在两个不同的压纹步骤中进行压纹。在单一步骤压纹中,使用两个压纹辊,而在多步骤压纹中,使用压纹辊和压辊(pressure roller)。压辊优选具有肖氏A硬度为20-80的橡胶表面。
用粗糙度值Rz量度所述膜的表面粗糙度根据DIN EN ISO 4287和DIN ISO 4288进行。用于测量表面粗糙度的测量设备必须满足EN ISO 3274。所用的轮廓滤波器必须符合DIN EN ISO 11562。
根据本发明的压纹步骤b)可以使得结构化膜的两个面具有不同粗糙度深度Rz的方式进行。例如,这可通过不同的压纹工具或压纹工具和/或压辊的温度来实现。
所述膜的两个表面上的槽可彼此成(share)70至90°或5-45°的角度。在另一方面,所述膜的至少一个表面上的槽相对挤出方向具有5-45°,优选35-45°的角度。
在所述膜的各表面上,槽的间距可相同或不同,所述表面之间的偏差为5%的情形视为相同。槽的间距可为100-1500 µm,优选300-1000 µm。
通过举例方式,图1显示了通过本发明方法制备的膜的表面,其具有500 µm的间距a)、75 µm的槽宽b)和40 µm的槽之间的隆起的表面粗糙度c)。
在压纹过程之前和/或之后,可将所述膜冷却至-10至+40℃以采取此方式固定膜的表面结构。冷却优选经由相应调温的冷却辊进行。
优选地,压纹辊由金属或陶瓷制成并具有带有后来存在于膜表面中的结构的负性轮廓图案的表面。优选压纹辊的槽的深度比膜的预期粗糙度高以在压纹后保持熔体破裂表面。
压纹辊的温度为80至200℃,尤其80至170℃,优选100至160℃且特别是110至155℃。特别优选地,压纹辊具有经涂布的钢表面(例如,用聚合物或陶瓷涂布),以降低膜的粘附。
在第一实施方案中,将挤出膜在具有相同或不同表面浮雕(embossment)的两个压纹辊之间压纹。
在本发明的另一实施方案中,在以相反方向旋转的压纹辊和压辊之间引导膜。优选地,在压纹辊之间和/或压纹辊和压辊之间,使膜暴露于10至400 N/mm,尤其10至150 N/mm,优选30 至130 N/mm并且特别地40至110 N/mm的线压力(line pressure)。如果进行若干个方法步骤b),则线压力可相同或不同。线压力是指基于膜宽的辊对(roller pair)的挤压力。
压辊优选具有0至50℃,优选5至30℃的温度,即它们面对压纹辊是有效冷却的(actively cooled)。在方法步骤b)中压辊的温度可相同或不同。
压辊将膜挤压入压纹辊的结构化表面中并轻轻地靠着压纹辊。通过改变线压力,可改变压纹区的表面以及因此膜在辊隙中的停留时间。
通过选择工艺参数——线压力、膜温度和/或辊温度、辊速度和膜幅(film web)在辊上的包角,膜压纹的粗糙度深度可受到压纹辊的给定粗糙度深度的影响。
在这种情况下,也可直接引导膜通过调温辊的辊隙,即不环绕通过它们。
可能特别使用交联或非交联形式的聚乙烯醇缩丁醛(PVB)作为与至少一种增塑剂、染料、颜料、用于粘附调节的金属盐、有机添加剂和/或无机填料混合的部分缩醛化的聚乙烯醇。
一方面,本领域已知用于此目的的所有增塑剂,特别是多价酸、多元醇或低聚醚二醇的酯,如,例如己二酸酯、癸二酸酯或邻苯二甲酸酯,特别是己二酸二正己酯、癸二酸二丁酯、邻苯二甲酸二辛酯,二甘醇、三甘醇或四甘醇与直链或支链脂肪族羧酸的酯以及这些酯的混合物适合作为部分缩醛化的聚乙烯醇的增塑剂。脂肪族二醇与长链脂肪族羧酸的酯,特别是三甘醇与包含6至10个碳原子的脂肪族羧酸(如 2-乙基丁酸或正庚酸)的酯优选用作部分缩醛化的聚乙烯醇,特别是聚乙烯醇缩丁醛的标准增塑剂。特别优选使用来自己二酸二正己酯(DHA)、癸二酸二丁酯(DBS)、邻苯二甲酸二辛酯(DOP),二甘醇、三甘醇或四甘醇与直链或支链脂肪族羧酸的酯,特别是双-2-乙基丁酸三甘醇酯(3GH)、双正庚酸三甘醇酯(3G7)、双-2-乙基己酸三甘醇酯(3G8)、双正庚酸四甘醇酯(4G7)中的一种或若干种增塑剂。
在本发明的一个特别实施方案中,可通过将减少粘附的物质加入膜材料进一步减少所述膜与压纹工具的粘附。
增塑的部分缩醛化的聚乙烯醇树脂优选包含25至45重量份且特别优选地30至40重量份的增塑剂,以100重量份的树脂为基计。
以已知的方式通过水解聚乙烯酯的缩醛化制备部分缩醛化的聚乙烯醇。甲醛、乙醛、丙醛、丁醛以及诸如此类,优选例如丁醛用作醛。
优选的聚乙烯醇缩丁醛树脂包含10至25重量%,优选17至23重量%并且特别优选19至21重量%的乙烯醇基团和/或0至20重量%,优选0.5至2.5重量%的乙酸酯基团。
在又一方法变型中,与多元醛(特别是戊二醛)和氧代羧酸(特别是乙醛酸)部分交联的PVB用作根据WO 2004/063231 A1的聚合物。这种部分交联的PVB具有比类似的非交联PVB的粘度高10至50%的粘度。
所述膜的水含量优选调节到0.15至0.8重量%,特别到0.3至0.5重量%。
根据本发明制备的膜可特别用于由一块或若干块玻璃板和/或一块或若干块聚合物板和至少一种结构化膜来制造层压件。
在这些层压件制造期间,首先通过挤压真空袋或真空环由所述玻璃/聚合物板和所述膜制备预复合材料(pre-composite)。通常,由于包含空气,预复合层压件稍微混浊。层压件的最终制造在高压釜中例如根据WO 03/033583进行。
实施例
根据本发明的实施例
通过以下条件挤出0.76 mm厚的包含38份增塑剂每100 份PVB 树脂的名义水平的PVB膜。
唇口温度:190℃。
熔体流动速率:1000 kg/h。
线速度:15m/min。
此PVB膜在各面上具有熔体破裂表面粗糙度,其特征在于熔体破裂Rz值为40微米。
在具有以下性质的设备中将此PVB膜压纹。两个压纹阶段的压辊和压纹辊具有相同的性质。
设备参数:
橡胶辊的硬度:70±5肖氏A
压纹辊的粗糙度:约200 m
压纹辊的间距:约500 m
槽的角度:12°
表面涂层:聚合物
橡胶辊的温度:10℃。
表1
膜的性质显示于以下表中,其中“Rz最终”代表压纹后的粗糙度,“Rz隆起”代表槽之间的隆起的粗糙度并且“槽深度”定义为“Rz最终–Rz隆起”。
表2
在复合玻璃制造期间,所述膜展示良好的除气性质并且能加工成无气泡的层压件。
对比实施例:
表3
在复合玻璃制造期间,所述膜展示差的除气性质并且不能加工成无气泡的层压件。
尤其是8号样品显示高粘着性。由于两层之间的高粘附/粘连,非常难以处理此膜。
采用本发明的方法可制备具有低粘连倾向的增塑聚乙烯醇缩醛膜。这种膜可卷绕到辊上用于运输并容易退卷(unroll)用于制备层压窗用玻璃(laminated glazing)。
Claims (11)
1.方法,用于通过以下方法步骤将包含增塑聚乙烯醇缩醛的膜压纹,以使在至少一个表面上的粗糙度Rz为20至100 µm:
a.将增塑聚乙烯醇缩醛挤出成所述表面的随机粗糙度Rz = 1至70 µm的膜,
b.将步骤a)中获得的所述膜的至少一个表面压上具有5-50 µm的深度、10- 200 µm的宽度和50 -2500 µm的间距的槽,其中
c.所述槽之间的隆起的所述表面粗糙度比步骤a)中所获得的低至多20%。
2.根据权利要求1的方法,其特征在于,用具有80至200℃温度的压纹辊将所述膜压纹。
3.根据权利要求1或2的方法,其特征在于,用10至400 N/mm的线压力将所述膜压纹。
4.根据权利要求1或2的方法,其特征在于,步骤a)中的所述增塑聚乙烯醇缩醛膜的所述挤出在熔体破裂条件下进行。
5.根据权利要求4的方法,其特征在于,所述在熔体破裂条件下的挤出采用具有100-270℃的唇口温度的挤出模头进行。
6.根据权利要求4的方法,其特征在于,所述在熔体破裂条件下的挤出采用500 - 3500kg/h的熔体流动速率进行。
7.根据权利要求1或2的方法,其特征在于,压纹的所述膜的两个表面具有相同的所述槽的间距。
8.根据权利要求1或2的方法,其特征在于,压纹的所述膜的两个表面具有不同的所述槽的间距。
9.根据权利要求1或2的方法,其特征在于,所述膜的两个表面上的所述槽彼此成70-90°的角度。
10.根据权利要求1或2的方法,其特征在于,所述膜的至少一个表面上的所述槽相对挤出方向具有5-45°的角度。
11.根据权利要求1或2的方法,其特征在于,在两个不同的压纹步骤中将所述膜的所述表面压纹。
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CN103481597A (zh) * | 2012-06-13 | 2014-01-01 | 可乐丽欧洲有限责任公司 | 用于复合玻璃件的压印塑料薄膜 |
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US20170266861A1 (en) | 2017-09-21 |
KR102265817B1 (ko) | 2021-06-15 |
EP3186059B1 (en) | 2018-11-28 |
WO2016030284A1 (en) | 2016-03-03 |
JP2017525597A (ja) | 2017-09-07 |
CN106660239A (zh) | 2017-05-10 |
JP6679571B2 (ja) | 2020-04-15 |
KR20170046726A (ko) | 2017-05-02 |
US10363696B2 (en) | 2019-07-30 |
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