CN113508159A - 经包装的粘弹性聚合物物质 - Google Patents
经包装的粘弹性聚合物物质 Download PDFInfo
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- CN113508159A CN113508159A CN201980087168.1A CN201980087168A CN113508159A CN 113508159 A CN113508159 A CN 113508159A CN 201980087168 A CN201980087168 A CN 201980087168A CN 113508159 A CN113508159 A CN 113508159A
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- Prior art keywords
- polymer
- viscoelastic
- protective
- strand
- acrylate
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- CXOYJPWMGYDJNW-UHFFFAOYSA-N naphthalen-2-yl 2-methylprop-2-enoate Chemical compound C1=CC=CC2=CC(OC(=O)C(=C)C)=CC=C21 CXOYJPWMGYDJNW-UHFFFAOYSA-N 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- MDYPDLBFDATSCF-UHFFFAOYSA-N nonyl prop-2-enoate Chemical compound CCCCCCCCCOC(=O)C=C MDYPDLBFDATSCF-UHFFFAOYSA-N 0.000 description 1
- NZIDBRBFGPQCRY-UHFFFAOYSA-N octyl 2-methylprop-2-enoate Chemical compound CCCCCCCCOC(=O)C(C)=C NZIDBRBFGPQCRY-UHFFFAOYSA-N 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
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- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
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- QIWKUEJZZCOPFV-UHFFFAOYSA-N phenyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1 QIWKUEJZZCOPFV-UHFFFAOYSA-N 0.000 description 1
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- RGBXDEHYFWDBKD-UHFFFAOYSA-N propan-2-yl propan-2-yloxy carbonate Chemical compound CC(C)OOC(=O)OC(C)C RGBXDEHYFWDBKD-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
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- 235000015096 spirit Nutrition 0.000 description 1
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- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- BWSZXUOMATYHHI-UHFFFAOYSA-N tert-butyl octaneperoxoate Chemical compound CCCCCCCC(=O)OOC(C)(C)C BWSZXUOMATYHHI-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B29/00—Packaging of materials presenting special problems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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Abstract
本发明涉及用于制造经包装的粘弹性聚合物物质的方法。本发明还涉及可根据本发明的方法获得的经包装的粘弹性聚合物物质、以及所述经包装的粘弹性聚合物物质用于在热和剪切的影响下进一步加工的用途。
Description
本发明涉及用于制造经包装的(经包裹的)粘弹性聚合物物质的方法。本发明还涉及可根据本文中描述的方法获得的经包装的粘弹性聚合物物质、以及所述经包装的粘弹性聚合物物质用于在热和剪切的影响下进一步加工的用途。
粘弹性聚合物物质是已知的并且经常用于制造胶粘剂组合物。相应的胶粘剂组合物包括例如聚丙烯酸酯聚合物,其常常经由聚合工艺在溶液中制备。当这样的基础聚合物的聚合在溶剂中进行时,在聚合物制备后通过除去溶剂而将聚合物浓缩。随后将聚合物与制造胶粘剂组合物所需的其他成分掺混。根据要设置的胶粘剂性质,基础聚合物的性质和成品胶粘剂组合物的各成分都可有大的变化(有很大差异)。为了使相应的聚合物物质的进一步加工尽可能灵活并且为了储存例如相对大量的基础聚合物、胶粘剂组合物前体或胶粘剂组合物本身,必须将相应的聚合物物质包装。
因此,需要提供可储存形式的粘弹性聚合物物质,其在需要时还可在规模工艺中用于进一步加工。
EP 3004272 B1致力于提供多种形式的经包装的胶粘剂例如垫子,并且描述了经包装的热熔性压敏胶粘剂,其包括热熔性压敏胶粘剂组合物和由如下组成的共挤出涂层:具有特定的熔体流动指数的纯聚乙烯、纯聚丙烯或纯乙烯-乙酸乙烯酯。根据现有技术,可通过如下方式制造自胶粘聚合物物质:将胶粘剂和保护性聚合物共挤出,之后将包封的聚合物分成多个部分。然而,迄今为止,不能可靠地用这种保护性聚合物包封适合用于制造自胶粘组合物的具有高分子量的粘弹性聚合物。一方面,为此所需的加工温度导致保护性聚合物的破坏;另一方面,在分离步骤期间在粘弹性聚合物内出现增加的内部压力,该压力在随后的储存时间期间消散并导致保护性聚合物封套在接缝处打开。结果是粘弹性聚合物的不希望的显露。
可借助于大量的保护性聚合物来对抗该风险。然而,为了最小化对粘弹性聚合物的性质的影响,非胶粘性的保护性聚合物的分数(比例)应尽可能小。较小分数的保护性聚合物导致上述对于外部机械和热载荷的敏感性。因此,任务是在保护性作用和对热熔性压敏胶粘剂的性质的影响之间找到平衡的折衷。
具有高分子量的粘弹性聚合物需要高的加工温度以使它们成为流体状态。高的加工温度存在如下的风险:非胶粘性的保护性聚合物以这样的方式熔融或被损坏,使得粘弹性聚合物显露并且不再能够进行进一步加工。因为保护性聚合物在再熔融时不被除去,而是与粘弹性聚合物一起形成塑化形式,所以不能使用具有相对高的软化点或熔点的保护性聚合物,因为这会导致可能的不允许的高的进一步加工温度,或未熔化的保护性聚合物的残留物将保留在粘弹性胶粘剂基质中。两种可能性都可对以后用作自胶粘组合物产生不希望的后果。
然而,特别是对于大量的经包装的胶粘剂和胶粘剂前体(其难以在室温下包装并且甚至在升高的温度下仍然具有100Pas或更高的高粘度),仍然需要改进。特别地,目前还缺乏允许简单有效地制造大量的经包装的粘弹性聚合物物质的合适的方法。在此的关键问题是用于包装的聚合物物质必须被加热和塑化(增塑)。因为大量的聚合物物质比少量的聚合物物质储存更多的热量,所以迄今为止大规模制造经包装的聚合物物质中的限制因素是先前为更好地加工而投入聚合物物质的热能的耗散(释放)。换句话说,必须再次释放在包装之前为更好地塑化而加热聚合物物质所采用的能量。
由此可推断,在大量的经包装的粘弹性聚合物物质的情况下,需要折衷。这种折衷包括冷却大量聚合物物质所花费的大量时间。或者必需制造大量的其内容物可被快速冷却的独立包装。然而,这种方法存在问题,因为特别是在大量的小的独立包装的情况下,存在一些小的包装的保护封套打开的风险,结果是可能阻塞并粘到其他小的包装上。
因此,仍然需要有效且快速的用于提供大量的经包装的粘弹性聚合物物质的方法。特别地,需要有效且快速的用于提供大量的经包装的基础聚合物的方法,所述经包装的基础聚合物基本上由聚(甲基)丙烯酸酯组成并可用作热熔性压敏胶粘剂。相应的基础聚合物首先在溶剂中制备,优选地通过自由基聚合方法,随后在热和真空的影响下在浓缩过程中除去溶剂。如果如此制备的基础聚合物仍然不适合作为自胶粘热熔性压敏胶粘剂,则在一个或多个下游步骤中将这些基础聚合物与其他添加剂例如增粘树脂、填料、增塑剂、交联剂等共混。基础聚合物的这种所谓的配混优选连续地在双螺杆挤出机中或在行星辊挤出机中进行。
进一步的需要是提供这样的方法,该方法使得粘弹性聚合物物质、特别地基础聚合物能够在没有用于其聚合或浓缩的设施的地方处进行加工。因此,任务是找到一种程序,通过该程序,粘弹性基础聚合物可被运输并且在预定位置处被共混以形成热熔性压敏胶粘剂组合物。
一种用于储存和运输可熔融聚合物例如热熔性胶粘剂的已知且经常使用的方法包括将它们装入(分配到)光滑壁的桶中,在其中聚合物在其储存和其运输之后首先借助于所谓的鼓式熔化器(鼓式胶机)进行加热以增加聚合物物质的流动性,然后将聚合物物质供应至进一步的操作。在高粘度的粘弹性基础聚合物的情况下,这种储存形式仅在极其昂贵和不便的条件下才有可能,因为高粘度意味着仅达到低熔体流速,因此使制造过程不经济。
针对该背景,本发明所要解决的问题是提供用于制造可以大的量运输和储存的经包装的粘弹性聚合物物质的方法,其中该方法可以减少的时间花费来完成,并且避免独立包装的粘连和阻塞。
本发明借助于如下的用于制造经包装的粘弹性聚合物物质的方法解决该问题,所述方法包括以下步骤:
a)在升高的温度下提供和塑化粘弹性聚合物物质,其中所述聚合物物质是基于具有500 000g/mol或更高的重均分子量的聚(甲基)丙烯酸酯的聚合物物质;
b)将经塑化的粘弹性聚合物物质连续分配(填充)到保护性聚合物膜中,以获得具有55至70mm直径的股状(线状)聚合物组件(聚合物复合物),该保护性聚合物膜没有自胶粘性质并且在用粘弹性聚合物物质填充之前已制成管状形式,该股状聚合物组件包括经塑化的粘弹性聚合物物质的芯和保护性聚合物膜的壳,其中基于保护性聚合物膜和粘弹性聚合物物质的总重量,保护性聚合物膜的分数小于1.0重量%,并且其中经塑化的粘弹性聚合物物质在被分配到管状保护性聚合物膜中的时间点具有大于100Pas的粘度;
c)将股状聚合物组件转变为扁平的(整平的,压平的)股状聚合物组件,其最小横截面具有约2:1至7:1、优选地约3:1至5:1的宽高比;
d)将扁平的股状聚合物组件冷却至该聚合物组件仍能塑性变形时的温度;
e)并且随后将扁平的股状聚合物组件卷绕在卷轴上,其中卷绕在卷轴上的股状聚合物组件具有超过30米的长度、优选地超过50米的长度、和更优选地超过100米的长度。
在本发明的方法中,还在进入冷却浴之前,将粘弹性聚合物和保护性聚合物的组件压平(整平),优选地借助于辊,以实现粘弹性聚合物的更快速的冷却以及因此的保护性聚合物的热保护。
本发明另外涉及能通过本文中描述的方法获得的经包装的粘弹性聚合物物质,以及如本文中描述的经包装的粘弹性聚合物物质在进一步加工操作中的用途和应用。在该用途的一种优选的实施方式中,将包覆有保护性聚合物的粘弹性基础聚合物置于塑化状态以进行进一步加工,并且加热至如下的温度:在该温度下,保护性聚合物熔融并被均匀地引入到粘弹性基础聚合物中。
在本文中描述的方法的步骤a)中,提供并在升高的温度下塑化粘弹性聚合物物质,然后将经塑化的聚合物物质连续分配到保护性聚合物膜中。粘弹性聚合物物质是基于具有500 000g/mol或更高的重均分子量的聚(甲基)丙烯酸酯的聚合物物质,并且在被分配到管状保护性聚合物膜中的时间点具有大于100Pas的粘度。
在本发明的意义上,“塑化”是指达到如下的状态:在该状态下粘弹性聚合物物质是可变形的,优选可流动的。在用于塑化的升高的温度下,与在未升高的温度的情形下的情况相比,聚合物物质在此具有更好的可变形性,换言之,增加的可流动性。粘弹性聚合物物质的塑化优选在升高的温度下在挤出机中进行。
此外,在被分配到管状形式中的时间点,粘弹性聚合物物质具有大于100Pas的粘度。使用来自Rheometric Scientific Incorporation的ARES流变仪(空气轴承(luftgelagert))(几何类型=平行板;直径=25.0[mm];测试类型=速率扫描;温度=100;120;140;160;180[℃];扫描模式=log;初始速率=0.1[1/s];最终速率=100.0[1/s];每十倍范围的点数=[6])测定粘度。
在本文中描述的方法的步骤b)中,将来自步骤a)的经塑化的粘弹性聚合物物质连续分配到保护性聚合物膜中。保护性聚合物膜由不具有自胶粘性质的保护性聚合物组成。在填充之前,保护性聚合物膜被制成管状形式。因此管状保护性聚合物膜不是通过共挤出工艺获得的;而是,从常规膜开始,产生管状形式。这是可能的,例如,通过从幅面形式的膜开始将该膜的两个相反的侧边缘以形成管的方式彼此连接。侧边缘的连接可借助于热引入和压力进行。
在步骤b)中,通过将粘弹性聚合物物质分配到管状保护性聚合物膜中得到股状聚合物组件,其包括经塑化的粘弹性聚合物物质的芯和保护性聚合物的壳。基于保护性聚合物和粘弹性聚合物物质的总重量,根据本发明的保护性聚合物的分数小于1.0重量百分比。在本文中描述的步骤a)和b)中,于是产生股状聚合物组件。该股状聚合物组件具有约55-70mm、优选地60-70mm的直径,其中由于在步骤b)中填充的保护性聚合物膜的管状形式,直径初始是圆形的。
在步骤c)中,然后将股状聚合物组件制成扁平的股状聚合物组件,其最小横截面具有约2:1至7:1、优选地约3:1至5:1的宽高比。在本上下文中,表述“最小横截面”是指在垂直于股状聚合物组件的纵轴的平面中进行测量。换句话说,不是基于沿聚合物股的最长延伸部分的横截面的测量,而是对与来自步骤b)的股状聚合物组件的初始圆形横截面形式的偏差进行测定。最小横截面和宽高比是扁平程度的表达。可通过如下方式实现压平:引导股状聚合物组件通过辊隙或辊,例如旋转辊。在本发明的一种优选的实施方式中,压平借助于辊进行。
将股状聚合物组件转变为相应扁平的股状聚合物组件大大地改善了股状聚合物组件与其周围环境之间的热交换,使得步骤d),即股状聚合物组件的冷却可显著更快速地进行(与未压平的、基本上圆形的横截面形式相比)。在步骤d)中,将步骤c)中获得的扁平的股状聚合物组件冷却至聚合物组件仍可塑性变形时的温度。对于冷却,可将股状聚合物组件引导通过用作冷却段的水浴。在步骤d)结束时,扁平的股状聚合物组件的芯温度优选低于100摄氏度,优选地低于90摄氏度,更优选地低于80摄氏度。芯温度的术语在本发明中理解为在股状聚合物组件的横截面中心的温度。
在本文中描述的方法的步骤e)中,随后将股状聚合物组件卷绕在卷轴上,其中卷绕在卷轴上的股状聚合物组件具有超过30米、优选地超过50米、和更优选地超过100米的长度(在未卷绕状态下)。
在根据本发明的一种特别优选的方法中,首先将步骤d)中获得的股状聚合物组件在步骤e)开始时引导通过卷轴端面中的开口并固定在那里。这确保在初始卷绕到卷轴上的端部的区域中,股状聚合物组件不滑动并且聚合物物质不从保护性聚合物封套中显露。
本文中描述的本发明的方法的特别有利的实施方式使用这样的粘弹性聚合物物质,其在转变为股状形式时具有大于250Pas的粘度、优选地大于500Pas的粘度。
本发明中使用的保护性聚合物膜优选包括聚乙烯、聚丙烯、乙烯-乙酸乙烯酯或其混合物。基于保护性聚合物和粘弹性聚合物物质的总重量,步骤b)中使用的保护性聚合物膜的分数更优选地小于0.8重量%、仍优选地小于0.5重量%,基于保护性聚合物和粘弹性聚合物物质的总重量。基于保护性聚合物和粘弹性聚合物物质的总重量,保护性聚合物的特别合适的分数位于0.05重量%至1重量%的范围内,优选在0.1重量%至0.8重量%的范围内,更优选在0.2重量%至0.5重量%的范围内,例如在0.25重量%至0.45重量%的范围内。
在本发明的另外的优选实施方式中,粘弹性聚合物物质为胶粘剂组合物(或其前体),优选地压敏胶粘剂组合物(或其前体)。本发明将术语“前体”理解为指粘弹性聚合物物质可用于制造胶粘剂组合物。通过本发明的方法包装的粘弹性聚合物物质特别优选地为胶粘剂组合物、理想地基础聚合物的前体。更特别地,就本发明的目的而言,胶粘剂组合物的前体优选地意指压敏胶粘剂组合物的前体。这样的前体可为在用作粘弹性聚合物物质的基础聚合物的聚合物的聚合结束时存在的聚合物。压敏胶粘剂组合物的前体的术语同样包括在将各种添加剂或组分添加至基础聚合物后获得的混合物。如本文中使用的压敏胶粘剂组合物的术语与自胶粘组合物的术语或压敏胶粘剂的术语同义。
压敏胶粘剂(PSA)或压敏胶粘剂组合物在本发明中按照通常的说法被理解为至少在室温下是永久粘性以及胶粘性的材料。PSA的特征是,可通过压力将它施加到基材并在那里保持粘附,其中无需详细地限定要施加的压力和暴露于该压力的时间。通常,尽管原则上取决于PSA和基材的精确性质、以及温度和大气湿度,但短时间暴露于最小压力(其不超出短暂温和接触)足以达到粘附效果,而在其他情况下,长时间暴露于较高压力也可为必要的。
在本发明的意义上,粘弹性聚合物物质为基于具有500 000g/mol的重均分子量的聚(甲基)丙烯酸酯的聚合物物质。
“聚(甲基)丙烯酸酯”是能通过丙烯酸类和/或甲基丙烯酸类单体以及任选的另外的可共聚单体的自由基聚合获得的聚合物。更特别地,“聚(甲基)丙烯酸酯”是其单体基础在达到至少50重量%的程度上由丙烯酸、甲基丙烯酸、丙烯酸酯和/或甲基丙烯酸酯组成的聚合物,其中至少部分地包括丙烯酸酯和/或甲基丙烯酸酯,优选地达到至少30重量%的程度,基于所讨论的聚合物的总单体基础。
本文中描述的粘弹性聚合物物质优选为压敏胶粘剂组合物或其前体,其中压敏胶粘剂组合物包括聚(甲基)丙烯酸酯,优选地以总共40至70重量%、更优选地以总共45至60重量%,在各自的情况下基于压敏胶粘剂组合物的总重量。可存在一种(单一的)聚(甲基)丙烯酸酯或多种聚(甲基)丙烯酸酯。
所述的压敏胶粘剂组合物的聚(甲基)丙烯酸酯的玻璃化转变温度优选地<0℃,更优选地在-20和-50℃之间。聚合物或嵌段共聚物中的聚合物嵌段的玻璃化转变温度在本发明中借助于动态扫描量热法(DSC)测定。为此,将约5mg未处理的聚合物样品称量到铝坩埚(体积25μl)中并用穿孔盖封闭。使用来自Netzsch的DSC 204F1进行测量。出于惰性化的目的在氮气下操作。将样品线冷却至-150℃,然后以10K/分钟的加热速率加热至+150℃,并且再次冷却至-150℃。随后的第二次加热曲线以10K/分钟再次运行,并且记录热容的变化。玻璃化转变被认为是热谱图中的台阶。
本文中描述的压敏胶粘剂组合物的聚(甲基)丙烯酸酯优选地包括至少一种部分共聚的官能单体、更优选地与环氧基团呈反应性以形成共价键的单体。非常优选地,部分共聚的官能单体、更优选地与环氧基团呈反应性以形成共价键的单体含有至少一个选自如下的官能团:羧酸基团、磺酸基团、膦酸基团、羟基基团、酸酐基团、环氧基团和氨基基团;更特别地,它包括至少一个羧酸基团。非常优选地,本文中描述的压敏胶粘剂组合物的聚(甲基)丙烯酸酯包括部分共聚的丙烯酸和/或甲基丙烯酸。所有提及的基团具有与环氧基团的反应性,因此使聚(甲基)丙烯酸酯有利地适于与引入的环氧化物热交联。
本文中描述的压敏胶粘剂组合物的聚(甲基)丙烯酸酯可优选地得自以下单体组成:
a)至少一种下式(1)的丙烯酸酯和/或甲基丙烯酸酯
CH2=C(RI)(COORII) (1),
其中RI=H或CH3并且RII为具有4-18个碳原子的烷基基团;
b)至少一种烯属不饱和单体,其具有至少一个选自如下的官能团:羧酸基团、磺酸基团、膦酸基团、羟基基团、酸酐基团、环氧基团和氨基基团;
c)任选的另外的丙烯酸酯和/或甲基丙烯酸酯和/或可与组分(a)共聚的烯属不饱和单体。
如下是特别有利的:选择具有45-99重量%的分数的组分a)的单体、具有1-15重量%的分数的组分b)的单体、和具有0-40重量%的分数的组分c)的单体,其中所述数字基于用于没有添加可能的添加剂例如树脂等的基础聚合物的单体混合物。
组分a)的单体通常是塑化的相对非极性的单体。更优选地,单体a)中的RII是具有4至10个碳原子的烷基基团或丙烯酸2-丙基庚酯或甲基丙烯酸2-丙基庚酯。式(1)的单体更特别地选自丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸正戊酯、甲基丙烯酸正戊酯、丙烯酸正戊酯、丙烯酸正己酯、甲基丙烯酸正己酯、丙烯酸正庚酯、丙烯酸正辛酯、甲基丙烯酸正辛酯、丙烯酸正壬酯、丙烯酸异丁酯、丙烯酸异辛酯、甲基丙烯酸异辛酯、丙烯酸2-乙基己酯、甲基丙烯酸2-乙基己酯、丙烯酸2-丙基庚酯和甲基丙烯酸2-丙基庚酯。
组分b)的单体更优选地选自丙烯酸,甲基丙烯酸,衣康酸,马来酸,富马酸,巴豆酸,乌头酸,二甲基丙烯酸,β-丙烯酰氧基丙酸,三氯丙烯酸,乙烯基乙酸,乙烯基膦酸,马来酸酐,丙烯酸羟乙酯、特别地丙烯酸2-羟基乙酯,丙烯酸羟丙酯、特别地丙烯酸3-羟基丙酯,丙烯酸羟丁酯、特别地丙烯酸4-羟基丁酯,丙烯酸羟己酯、特别地丙烯酸6-羟基己酯,甲基丙烯酸羟乙酯、特别地甲基丙烯酸2-羟基乙酯,甲基丙烯酸羟丙酯、特别地甲基丙烯酸3-羟基丙酯,甲基丙烯酸羟丁酯、特别地甲基丙烯酸4-羟基丁酯,甲基丙烯酸羟己酯、特别地甲基丙烯酸6-羟基己酯,烯丙醇,丙烯酸缩水甘油酯,甲基丙烯酸缩水甘油酯。
说明性的组分c)的单体为:
丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、丙烯酸苄酯、甲基丙烯酸苄酯、丙烯酸仲丁酯、丙烯酸叔丁酯、丙烯酸苯酯、甲基丙烯酸苯酯、丙烯酸异冰片酯、甲基丙烯酸异冰片酯、丙烯酸叔丁基苯酯、甲基丙烯酸叔丁基苯酯、甲基丙烯酸十二烷基酯、丙烯酸异癸酯、丙烯酸月桂酯、丙烯酸正十一烷基酯、丙烯酸硬脂基酯、丙烯酸十三烷基酯、丙烯酸二十二烷基酯、甲基丙烯酸环己酯、甲基丙烯酸环戊酯、丙烯酸苯氧基乙酯、甲基丙烯酸苯氧基乙酯、甲基丙烯酸2-丁氧基乙酯、丙烯酸2-丁氧基乙酯、丙烯酸3,3,5-三甲基环己酯、丙烯酸3,5-二甲基金刚烷基酯、甲基丙烯酸4-枯基苯酯、丙烯酸氰乙酯、甲基丙烯酸氰乙酯、丙烯酸4-联苯酯、甲基丙烯酸4-联苯酯、丙烯酸2-萘酯、甲基丙烯酸2-萘酯、丙烯酸四氢糠酯、丙烯酸二乙基氨基乙酯、甲基丙烯酸二乙基氨基乙酯、丙烯酸二甲基氨基乙酯、甲基丙烯酸二甲基氨基乙酯、3-甲氧基丙烯酸甲酯、丙烯酸3-甲氧基丁酯、甲基丙烯酸2-苯氧基乙酯、甲基丙烯酸丁基二甘醇酯、丙烯酸乙二醇酯、单甲基丙烯酸乙二醇酯、甲氧基聚乙二醇甲基丙烯酸酯350、甲氧基聚乙二醇甲基丙烯酸酯500、单甲基丙烯酸丙二醇酯、甲基丙烯酸丁氧基二甘醇酯、甲基丙烯酸乙氧基三甘醇酯、丙烯酸八氟戊酯、甲基丙烯酸八氟戊酯、甲基丙烯酸2,2,2-三氟乙酯、丙烯酸1,1,1,3,3,3-六氟异丙酯、甲基丙烯酸1,1,1,3,3,3-六氟异丙酯、甲基丙烯酸2,2,3,3,3-五氟丙酯、甲基丙烯酸2,2,3,4,4,4-六氟丁酯、丙烯酸2,2,3,3,4,4,4-七氟丁酯、甲基丙烯酸2,2,3,3,4,4,4-七氟丁酯、甲基丙烯酸2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-十五氟辛酯、二甲基氨基丙基丙烯酰胺、二甲基氨基丙基甲基丙烯酰胺、N-(1-甲基十一烷基)丙烯酰胺、N-(正丁氧基甲基)丙烯酰胺、N-(丁氧基甲基)甲基丙烯酰胺、N-(乙氧基甲基)丙烯酰胺、N-(正十八烷基)丙烯酰胺;N,N-二烷基取代的酰胺如N,N-二甲基丙烯酰胺和N,N-二甲基甲基丙烯酰胺;N-苄基丙烯酰胺、N-异丙基丙烯酰胺、N-叔丁基丙烯酰胺、N-叔辛基丙烯酰胺、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、丙烯腈、甲基丙烯腈;乙烯基醚如乙烯基甲基醚、乙基乙烯基醚、乙烯基异丁基醚;乙烯基酯如乙酸乙烯酯;乙烯基卤化物、亚乙烯基卤化物、乙烯基吡啶、4-乙烯基吡啶、N-乙烯基邻苯二甲酰亚胺、N-乙烯基内酰胺、N-乙烯基吡咯烷酮、苯乙烯、α-甲基苯乙烯和对甲基苯乙烯、α-丁基苯乙烯、4-正丁基苯乙烯、4-正癸基苯乙烯、3,4-二甲氧基苯乙烯;大分子单体如2-聚苯乙烯甲基丙烯酸乙酯(4000-13 000g/mol的重均分子量Mw,通过GPC测定)、聚(甲基丙烯酸甲酯)甲基丙烯酸乙酯(2000-8000g/mol的Mw)。
组分c)的单体还可有利地选择成使得它们含有支持随后的辐射-化学交联(例如,通过电子束、UV)的官能团。合适的可共聚光引发剂是例如丙烯酸苯偶姻酯和丙烯酸酯官能化的二苯甲酮衍生物。支持通过电子束轰击交联的单体是例如丙烯酸四氢糠酯、N-叔丁基丙烯酰胺和丙烯酸烯丙酯。
聚(甲基)丙烯酸酯优选通过常规自由基聚合或受控自由基聚合制备。聚(甲基)丙烯酸酯可通过如下方式制备:使用惯常的聚合引发剂以及任选的链转移剂使单体共聚,其中聚合在惯常温度下在本体中(以本体)、在乳液中(例如在水或液体烃中)或在溶液中进行。
聚(甲基)丙烯酸酯优选通过如下方式制备:在溶剂中、更优选地在具有50-150℃、更特别地60-120℃的沸程的溶剂中使用0.01-5重量%的聚合引发剂、更特别地0.1-2重量%的聚合引发剂使单体共聚,在各自的情况下基于单体的总重量。
所有惯常的引发剂原则上是合适的。自由基源的实例是过氧化物、氢过氧化物和偶氮化合物,例如过氧化二苯甲酰、氢过氧化枯烯、过氧化环己酮、过氧化二叔丁基、过氧化环己基磺酰基乙酰基、过碳酸二异丙酯、过辛酸叔丁酯和苯频哪醇。优选的自由基引发剂是2,2'-偶氮双(2-甲基丁腈)(来自DuPont的67TM)或2,2'-偶氮双(2-甲基丙腈)(2,2'-偶氮二异丁腈;AIBN;来自DuPont的64TM)。
优选的用于制备聚(甲基)丙烯酸酯的溶剂是醇例如甲醇、乙醇、正丙醇和异丙醇、正丁醇和异丁醇,特别地异丙醇和/或异丁醇;烃例如甲苯以及特别地具有60-120℃的沸程的矿物精(汽油);酮,特别地丙酮、甲乙酮、甲基异丁基酮;酯例如乙酸乙酯;和上述溶剂的混合物。特别优选的溶剂是以2-15重量%、更特别地3-10重量%的量包含异丙醇的混合物,在各自的情况下基于所用的溶剂混合物。
在使用溶剂的情况下,在制备聚(甲基)丙烯酸酯之后(即,在聚合结束时),存在浓缩过程,并且将如此产生的聚合物以基本上无溶剂的形式作为粘弹性聚合物物质用于本发明的方法中。
可在不存在另外的添加剂如交联剂和促进剂物质的情况下进行聚合物的浓缩。然而,也可甚至在浓缩之前添加这些类别的化合物之一,从而浓缩在所述物质的存在下进行。然而,只有当所选择的添加剂的存在不违背本发明的方法这才是有意义的,因为根据本发明,首先提供并在升高的温度下塑化粘弹性聚合物物质(步骤a)),然后将基于聚(甲基)丙烯酸酯的经塑化的粘弹性聚合物物质填充到保护性聚合物膜中(步骤b))。因此,在本发明中,如果添加剂与各个方法步骤的温度不相容,则不将添加剂添加至所述方法的各步骤中。
在本发明中,聚(甲基)丙烯酸酯的重均分子量Mw为500 000g/mol或更高、优选地750 000g/mol或更高、更优选地1 000 000g/mol或更高。为此,如下可为有利的:在合适的聚合链转移剂如硫醇、卤素化合物和/或醇的存在下进行聚合,以建立期望的平均分子量。
本文中的重均分子量Mw(以及同样地数均分子量Mn)的数字基于通过凝胶渗透色谱法(GPC)的已知测定。该测定是对已经经历澄清过滤的100μl样品(样品浓度4g/l)进行的。使用的洗脱液是具有0.1体积%三氟乙酸的四氢呋喃。测量在25℃下进行。
使用的预柱是PSS-SDV柱,5μm,8.0mm*50mm(在此和下面的细节是按以下顺序:类型,粒度,孔隙率,内径*长度;)。使用如下的组合进行分离:PSS-SDV柱,5μm,以及和各自具有8.0mm*300mm(来自Polymer StandardsService的柱;使用Shodex RI71差示折射仪的检测)。流速为1.0ml/分钟。在聚(甲基)丙烯酸酯的情况下对照PMMA标准物进行校正(聚甲基丙烯酸甲酯校正),并且在其它情况(树脂、弹性体)下对照PS标准物进行校正(聚苯乙烯校正)。
在本发明中,基于聚(甲基)丙烯酸酯的粘弹性聚合物物质是包括一种或多种聚(甲基)丙烯酸酯或者由一种或多种聚(甲基)丙烯酸酯组成的聚合物物质。本发明的特别优选的实施方式涉及其中粘弹性聚合物物质为自胶粘组合物或可转变为自胶粘组合物的方法。
本发明理解术语“可转变”是指例如如下的情况:其中粘弹性聚合物物质可通过改性、例如通过交联和/或通过添加添加剂而转变为实际的压敏胶粘剂组合物。取决于所需的交联度,可已经以交联的聚(甲基)丙烯酸酯的形式提供粘弹性聚合物物质,或者仅在经包装的粘弹性聚合物物质在用于在热和剪切的影响下进一步加工的本文中的用途中使用时才进行用于建立所需的交联度的最后(结束的)交联。
如果在交联步骤之后需要具有相对低的分子量和良好的剪切强度的压敏胶粘剂组合物时,则本文中描述的聚合物物质的聚(甲基)丙烯酸酯可具有例如PD<4的多分散性和因此相对窄的分子量分布。而且,较低的多分散性使得能够更容易地从熔体加工,因为流体粘度低于具有基本上相同的应用性质的更宽分布的聚(甲基)丙烯酸酯的流体粘度。窄分布的聚(甲基)丙烯酸酯可有利地通过阴离子聚合或通过受控的自由基聚合技术制备,后者是特别合适的。相应的聚(甲基)丙烯酸酯也可经由N-氧基制备。另外,以有利的方式,可使用原子转移自由基聚合(ATRP)以合成窄分布的聚(甲基)丙烯酸酯,其中使用的引发剂优选包括单官能或双官能的仲或叔卤化物,并且为了提取卤化物使用Cu、Ni、Fe、Pd、Pt、Ru、Os、Rh、Co、Ir、Ag或Au的络合物。RAFT聚合也是合适的。
本文中描述的压敏胶粘剂组合物的聚(甲基)丙烯酸酯优选地通过它们含有的官能团与热交联剂的连接反应(尤其在加成或取代反应的意义上)来交联。可使用这样的所有热交联剂:其
-既确保足够长的处理时间,使得在处理操作、尤其是挤出程序期间没有胶凝,
-又导致聚合物在低于处理温度的温度下、更特别地在室温下快速后交联至期望的交联度。
例如,可能的是含有羧基、氨基和/或羟基的聚合物与作为交联剂的异氰酸酯、特别地脂族或封端的异氰酸酯、例如用胺失活的三聚异氰酸酯的组合。合适的异氰酸酯特别地为MDI[4,4-亚甲基二(苯基异氰酸酯)]、HDI[六亚甲基二异氰酸酯,1,6-亚己基二氰酸酯]和IPDI[异佛尔酮二异氰酸酯,5-异氰酸合-1-异氰酸合甲基-1,3,3-三甲基环己烷]的三聚衍生物,例如产品N3600和XP2410(分别来自BAYER AG:脂族多异氰酸酯,低粘度HDI三聚体)。同样合适的是微粉化的三聚IPDI(现在的 )(BAYERAG)的表面失活的分散体。
优选使用0.1-5重量%、更特别地0.2-1重量%的热交联剂,基于待交联的聚合物的总量。
还可经由络合剂(也称为螯合物)交联。优选的络合剂的实例是乙酰丙酮铝。
本文中描述的压敏胶粘剂组合物优选包括至少一种与聚(甲基)丙烯酸酯相容的增粘剂(其也可称为粘合力增强剂或增粘树脂)。符合本领域技术人员的一般理解的“增粘剂”是这样的低聚物型或聚合物型树脂:与不含增粘剂但在其它方面相同的压敏胶粘剂组合物相比,其提高压敏胶粘剂组合物的自粘附性(粘性,固有粘着性)。“与聚(甲基)丙烯酸酯相容的增粘剂”是指如下的增粘剂:与纯的聚(甲基)丙烯酸酯相比,其改变在聚(甲基)丙烯酸酯和增粘剂的充分混合后获得的体系的玻璃化转变温度,其中聚(甲基)丙烯酸酯和增粘剂的混合物也可分配仅一个Tg。在聚(甲基)丙烯酸酯和增粘剂的充分混合后获得的体系中,与聚(甲基)丙烯酸酯不相容的增粘剂将导致两个Tg,一个可分配给聚(甲基)丙烯酸酯且另一个可分配给树脂畴。在本上下文中,借助于DSC(差示扫描量热法)以量热的方式进行Tg的测定。
与聚(甲基)丙烯酸酯相容的增粘剂优选具低于0℃、非常优选地至多20℃的DACP,和/或优选地低于40℃、非常优选地至多20℃的MMAP。为了测定DACP和MMAP值,参考C.Donker,PSTC Annual Technical Seminar,Proceedings,第149-164页,2001年5月。
与聚(甲基)丙烯酸酯相容的增粘剂更优选为萜烯-酚醛树脂或松香衍生物,更特别地萜烯-酚醛树脂。本文中描述的压敏胶粘剂组合物还可包括两种或更多种增粘剂的混合物。在松香衍生物中,松香酯是优选的。
如本文中所述的压敏胶粘剂组合物优选包括总共7-25重量%、更优选地总共12-20重量%的与聚(甲基)丙烯酸酯相容的增粘剂,在各自的情况下基于压敏胶粘剂组合物的总重量。
取决于所描述的压敏胶粘剂组合物的应用领域和期望性质,它可包括在各自的情况下单独的或与一种或多种其他添加剂或组分组合的另外的组分和/或添加剂。
例如,本文中所述的压敏胶粘剂组合物可包括粉状和颗粒状的(特别地,还有耐磨的和增强的)填料、染料和颜料如二氧化钛、氧化锌和/或炭黑。此外,可存在各种有机填料。
粘弹性聚合物物质的密度优选为1.05-1.3g/cm3、更优选地1.10-1.25g/cm3,其在25摄氏度下测量。
如上所述,本发明首先提供粘弹性聚合物物质(步骤a))并且将其连续地填充到管状保护性聚合物膜中(步骤b)),然后将如此获得的股状聚合物组件压平(步骤c))并且随后进行冷却(步骤d))。为了将扁平的(压平的)股状聚合物组件卷绕到卷轴上(步骤e)),可使用适合于容纳相应长度的股状聚合物组件的任何期望的卷轴。
将股状聚合物组件卷绕到卷轴上确保可保持足够大量的粘弹性聚合物物质以备运输和储存。
在本发明的一种优选实施方式中,本文中描述的方法连续地进行。这意味着步骤a)至e)以这样的方式进行,使得在步骤d)之后,即在冷却之后,聚合物组件直接卷绕到卷轴上。为此,在实际的卷绕程序开始之前,可首先引导股状聚合物组件的一端通过卷轴端面中的开口并固定在那里。一旦足够长度的股状聚合物组件(即,至少30m、优选地50m或更多、更优选地100m或更多)已经卷绕在卷轴上,则股状聚合物组件的端部被闭合并且如果需要的话,固定在卷轴上。为了闭合股状聚合物组件,保护性聚合物可在其端部例如被胶粘粘合或焊接,例如通过分段地加热保护性聚合物并随后如热封工艺中已知的那样将它们对着彼此压制(压在一起)。
由此产生的粘弹性聚合物物质是本发明的主题且适合于使用和在热和剪切的影响下进一步加工。
因此,本发明提供这样的方法,利用该方法可位置独立地储存、运输和进一步加工大量的完成的聚合物物质。为此,例如,可从卷轴展开经包装的粘弹性聚合物物质并且将其连续引入挤出机中。在该挤出机中,然后将经包装的粘弹性聚合物物质在热和剪切的影响下塑化,并且优选地熔融,使得理想地保护性聚合物均匀地分布在粘弹性聚合物物质中。然后可将获得的粘弹性聚合物物质和保护性聚合物的混合物进行分配和/或成型,或者将粘弹性聚合物物质和保护性聚合物的混合物与其他添加剂掺混。
本文中描述的特定的量、尺寸和其他尺寸,例如保护性聚合物组分的量和扁平的股状聚合物组件的尺寸,允许简单地提供大量可运输和可储存的经包装的粘弹性聚合物物质,其中所述方法可以减少的时间花费来完成,并且避免独立包装的粘连和阻塞。同时确保在热和剪切的影响下进一步加工经包装的粘弹性聚合物物质以形成中间体或最终产品。为了与保护性聚合物一起进行进一步加工,有利地在热和剪切的影响下在挤出机中处理粘弹性聚合物物质。
已经显现,如本文中描述的将粘弹性聚合物物质连续分配到保护性聚合物膜中提供了稳定的股状聚合物组件,该组件可在-30℃至+60℃的温度范围内储存而不显露任何粘弹性聚合物物质。这使本发明的经包装的粘弹性聚合物物质区别于枕形的经包装的产品,在该枕形的经包装的产品中总是有单独的小包出现不希望的打开。此外,以本文中描述的量使用保护性聚合物确保,保护性聚合物在进一步加工中在热和剪切的影响下熔融并且可均匀地分布在粘弹性聚合物物质中。
Claims (15)
1.用于制造经包装的粘弹性聚合物物质的方法,包括如下的步骤:
a)提供和在升高的温度下塑化粘弹性聚合物物质,所述聚合物物质是基于具有500000g/mol或更高的重均分子量的聚(甲基)丙烯酸酯的聚合物物质;
b)将经塑化的粘弹性聚合物物质连续分配到保护性聚合物膜中,以得到具有55至70mm直径的股状聚合物组件,所述保护性聚合物膜没有自胶粘性质并且在用粘弹性聚合物物质填充之前已制成管状形式,所述股状聚合物组件包括经塑化的粘弹性聚合物物质的芯和保护性聚合物膜的壳,其中基于保护性聚合物膜和粘弹性聚合物物质的总重量,所述保护性聚合物膜的分数小于1.0重量%,并且其中所述经塑化的粘弹性聚合物物质在分配到管状保护性聚合物膜中的时间点具有大于100Pas的粘度;
c)将所述股状聚合物组件转变为扁平的股状聚合物组件,其最小横截面具有约2:1至7:1的宽高比;
d)将所述扁平的股状聚合物组件冷却至该聚合物组件仍能塑性变形时的温度;
e)并且随后将所述扁平的股状聚合物组件卷绕在卷轴上,其中卷绕在卷轴上的股状聚合物组件具有超过30米的长度。
2.如权利要求1所述的方法,其中步骤c)中的将所述股状聚合物组件转变为扁平的股状聚合物组件是借助于辊进行的。
3.如前述权利要求任一项所述的方法,其中步骤d)中的冷却进行至低于100℃的芯温度。
4.如前述权利要求任一项所述的方法,其中首先将步骤e)中的股状聚合物组件引导通过卷轴端面中的开口并且固定在那里。
5.如前述权利要求任一项所述的方法,其中步骤d)在水浴中进行。
6.如前述权利要求任一项所述的方法,其中步骤a)中的塑化在挤出机中进行。
7.如前述权利要求任一项所述的方法,其中所述经塑化的粘弹性聚合物物质在分配到管状保护性聚合物膜中的时间点具有大于250Pas的粘度。
8.如前述权利要求任一项所述的方法,其中基于保护性聚合物膜和粘弹性聚合物物质的总重量,步骤b)中的保护性聚合物膜的分数小于0.5重量%。
9.如前述权利要求任一项所述的方法,其中所述保护性聚合物膜由聚乙烯、聚丙烯、乙烯-乙酸乙烯酯或其混合物组成。
10.如前述权利要求任一项所述的方法,其中所述粘弹性聚合物物质为自胶粘组合物或可转变为自胶粘组合物。
11.如前述权利要求任一项所述的方法,其中所述粘弹性聚合物物质在25℃下具有1.05-1.3g/cm3的密度。
12.能通过权利要求1-11的方法获得的经包装的粘弹性聚合物物质。
13.如权利要求12所述的经包装的粘弹性聚合物物质在如下的方法中的用途:其中所述经包装的粘弹性聚合物物质通过在热和剪切的影响下进行塑化以用于进一步加工。
14.如权利要求13所述的用途,其中在用热和剪切处理所述经包装的粘弹性聚合物物质以用于进一步加工期间,同样将所述保护性聚合物膜塑化。
15.如权利要求13和14任一项所述的用途,其中用热和剪切处理在挤出机中进行。
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DE102018219357.6 | 2018-11-13 | ||
DE102018219357.6A DE102018219357A1 (de) | 2018-11-13 | 2018-11-13 | Verpackte viskoelastische Polymermasse |
PCT/EP2019/081138 WO2020099467A1 (de) | 2018-11-13 | 2019-11-13 | Verpackte viskoelastische polymermasse |
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CN (1) | CN113508159A (zh) |
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WO (1) | WO2020099467A1 (zh) |
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2019
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US20220010079A1 (en) | 2022-01-13 |
DE102018219357A1 (de) | 2020-05-14 |
EP3880750B1 (de) | 2023-01-04 |
WO2020099467A1 (de) | 2020-05-22 |
EP3880750A1 (de) | 2021-09-22 |
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