CN100518959C - 用行星式挤压机制备胶粘剂的工艺 - Google Patents

用行星式挤压机制备胶粘剂的工艺 Download PDF

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Publication number
CN100518959C
CN100518959C CNB2004800026203A CN200480002620A CN100518959C CN 100518959 C CN100518959 C CN 100518959C CN B2004800026203 A CNB2004800026203 A CN B2004800026203A CN 200480002620 A CN200480002620 A CN 200480002620A CN 100518959 C CN100518959 C CN 100518959C
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technology
planetary
mixer section
cementitious compositions
adhesive
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CN1832812A (zh
Inventor
小J·K·泰南
R·W·圣克尔
D·M·科瓦奇
T·隆巴尔多
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Intertape Polymer Corp
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Intertape Polymer Corp
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
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Abstract

描述了一种用改进的行星辊式挤压机制备压敏胶粘剂的工艺。根据本发明一个方面，该工艺包括：将包括非热塑性弹性体的初始原料引入改进的行星辊式挤压机的进料段；将原料从进料段传输到改进的行星辊式挤压机的混和段；在混和段里连续地混合初始原料，以制出均匀的粘性组合物。该粘性组合物可涂敷到片状材料上。改进的行星辊式挤压机的混和段包括有被多个行星心轴所包围并与之相啮合的主轴，其中至少行星心轴之一是具有多个顶部切槽螺齿的双横向混合心轴。

Description

用行星式挤压机制备胶粘剂的工艺
技术领域
本发明涉及一种用于非热塑性弹性体与增粘树脂素炼(mastication)和混合的连续低温工艺并且可包括下述中一个或多个料：热塑性弹性体、补充剂、增塑剂和油类、活化剂、抗降解剂、交联剂、着色剂、溶剂、以及发泡剂。在本发明的一个方面，胶粘剂可直接涂敷于片状(web-form)材料。
本发明总的目的是提供一种用于通过非热塑性弹性体在行星辊式挤压机(PRE)中素炼生产自粘性组合物的方法。在一个实施例中，素炼是通过使用双横向或者“顶部切槽”(back-cut)行星心轴结合全螺齿(full-flight)行星心轴来实现的，以便利用槽模(slot die)生产能适用于片状材料的胶粘剂。
背景技术
压敏胶粘剂组合物是几种原料的混合物，该原料包括弹性体、树脂、增塑剂以及比如抗氧化剂、填料、颜料等其它添加剂。由于这些组分必须以适当的比例进行混合，以获得具有所需性质的胶粘剂，原料通常在可控的条件下用机械搅拌器进行混合(作为分批工艺的一部分)，以获得原料相对含量适当的充分混合的产物。
行星辊式挤压机为人所共知，并且通常用于比如PVC之类的热塑性塑料的加工之中，例如这种挤压机曾主要用来供应下游装置，比如压延机或轧机。行星辊式挤压机通常用来加工具有最少降解的热敏混合物，因为薄层的混合物能暴露很大的表面，从而导致有效的热交换、混合和温度控制。行星辊式挤压机具有很多不同的结构和尺寸。根据所需的生产能力，辊筒的直径通常在70mm至500mm之间。
行星辊式挤压机通常具有装填段和混和段。装填段通常包括输送螺杆，一些原料连续地供应至该输送螺杆。然后，输送螺杆再将原料传送到混和段。混和段包括从动主轴和多个行星心轴，其在具有内螺旋齿轮装置的辊筒内绕着该主轴旋转。主轴的旋转速度以及由此行星心轴的旋转速度可以改变，并在混合工序期间作为一个可控的参数。原料在主轴和行星心轴之间循环，或者在行星心轴和辊段的螺旋齿轮装置之间循环，致使原料分散，从而形成均匀的组合物。
在每个辊筒中旋转的行星心轴的数目可以改变，并因而适应于这种加工的需要。心轴的数目影响行星辊式挤压机内的自由容积、原料在加工中的停留时间，并且还决定热和物料交换的表面面积。通过导入的分散能量，行星心轴的数目对混合的结果有影响。如果辊筒的直径恒定，较多数目的心轴便能带来更好的均化和分散作用，或者相应更高的产物生产量。
主轴和辊筒之间可安装最多数目的行星心轴取决于辊筒的直径和所用行星心轴的直径。如需要获得大规模的生产量而使用较大的辊径时，和/或行星心轴使用较小的直径时，辊筒可以装备较多数量的行星心轴。辊径为D＝70mm时，通常使用多达7个行星心轴，而当辊径为D＝200mm时，可使用例如10个行星心轴，而当辊径为D＝400mm时，则使用例如24个行星心轴。然而，这些例子无论如何对本领域的技术人员也不构成限制。例如，如果主轴的直径相对于较大的主轴较小，则可增加行星心轴的数目。
发明内容
本发明的目的在于使用一种改进的行星辊式挤压机制备胶粘剂的工艺。根据本发明一个方面，该工艺包括：将包括非热塑性弹性体的初始原料引入改进的行星辊式挤压机进料段；将原料从进料段传输到改进的行星辊式挤压机混和段；在混和段里混合初始原料，制出均匀的粘性组合物并将该粘性组合物涂敷于片状材料。改进的行星辊式挤压机混和段包括有被多个行星心轴所包围并与之相啮合的主轴，其中至少行星心轴之一是具有多个顶部切槽螺齿的双横向混合心轴。
根据本发明的另一方面，改进的行星辊式挤压机用于制造粘性组合物。根据本发明这个方面，该工艺包括：将包括非热塑性弹性体和增粘树脂的粘性组合物初始原料连续地计量进入行星辊式挤压机；在行星辊式挤压机混和段里连续地混合原料，以形成均匀的粘性组合物，其中混和段包括有被多个行星心轴所包围并与之相啮合的主轴，其中至少行星心轴之一是具有多个顶部切槽螺齿的双横向混合心轴；和将均匀的粘性组合物连续地从挤压机中排出。根据一些实施例，自粘性组合物可用比如槽模敷料器装置之类的敷料器装置涂敷于片状材料，并且随后交联。
根据本发明的另一方面，弹性体这样素炼，以使用GPC(凝胶渗透色谱法)测量时Mw减少至小于1,000,000。在本发明的其它方面，弹性体可素炼使得Mw减少超过约50％，更个别地超过约80％，相对于弹性体的原始Mw而言。
附图说明
以下结合附图更详细地描述本发明的典型实施例，其中：
图1是根据本发明一个方面的行星辊式挤压机纵截面图；
图2是典型双横向混合心轴的放大图；
图3是图1中行星辊式挤压机的定量环(dosing ring)横截面图；
图4是槽模涂料器的横截面图；
图5是根据本发明一个方面的行星辊式挤压机和槽模涂料器的纵截面图；
图6是图1行星辊式挤压机沿6-6线的横截面图。
具体实施方式
所有相关部分引用的文献均列入本专利作为参考；任何文献的引用都不应视作已经认可其相对于本发明为现有技术。
现在转向附图，并且首先参考图1，其中示出根据本发明一个实施例的行星辊式挤压机，通常用附图标记10标示。可以理解，行星辊式挤压机系统以示意形式示出，以便以更易于理解的方式描述其操作。然而，在实际实践中，系统10的形状和大小可能与所示的具有实质上的不同，但是仍然在本专利提出的权利要求范围内。
行星辊式挤压机系统10包括进料段12和混和段14。胶粘剂的初始原料添入进料喉部16并计量到装填段12的输送螺杆18上。本文使用的术语“初始原料”指的是添入行星辊式挤压机10进料段12里胶粘剂配方的那些材料。初始原料可包括，但并不限于弹性体、树脂、补充剂、活化剂、抗降解剂和交联剂。螺杆18将初始原料输入混和段14。如图1所示，混和段14包括四个被定量环22a、22b和22c分隔开的行星辊筒段20a、20b、20c和20d。每个辊筒段20包括45°螺齿的筒体24、45°螺齿的主轴26和多个45°螺齿的行星心轴28、30。螺旋齿轮装置可具有任何适当的角度，例如10至60°的角度，更个别地可使用稍大于20°的角度。根据本发明的一些方面，至少辊筒段20中之一包括双横向行星心轴28。本发明并不限于使用双横向行星心轴。也可使用其它达到预期混合水平的心轴构型。
行星心轴28、30的最多数目是主轴26和螺齿筒体24直径的函数。行星心轴28、30可示有很多不同的几何齿形，例如全螺齿(Planetspindel)30、双横向螺齿(也称作“顶部切槽”心轴或Noppenspindel)28、或分区螺齿(Igelspindel)等。所选行星心轴的数目和它们的几何形状(例如开式与全螺齿)可以这样控制，即影响每个辊筒段20的动态排出效果和各段之间的排出差异。另外，可以改变定量环22和主轴26之间的间隙，以改变每个筒段20的动态排出效果和各筒段20之间的排出差异。
标准的行星心轴30表示为筒体，其中的槽或螺齿与心轴轴线切成45°角(与主轴螺齿的角度相同)。行星心轴搭在主轴螺齿上运动，这样的结构使行星心轴28、30和主轴26产生相同的表面速度。在主轴和行星心轴之间具有间隙，其充满了加工物料，并且最终结果可在主轴26、行星心轴28、30以及筒壁24之间出现近似零剪切分布和分散混合。
成45°角切入行星心轴和主轴的另一最终结果是作用在加工物料上的正压力前进运动。采用双横向心轴28(也称作noppenspindles或顶部切槽心轴)是产生较低压力、较大滑动量、较少前进运动、更长停留时间，进而更强大混合的一种变型。
双横向行星心轴28是螺齿具有开口的心轴，这使物料能在筒24的壁和主轴26之间穿过，并且放慢物料经过行星辊式挤压机系统10的速度。双横向心轴28的一个例子是所谓的针式(porcupine)心轴。双横向心轴28的一个具体例子在图2中详细示出，顶部切槽开口32增长了停留时间并促进了混合。双横向心轴28的结构是标准行星心轴的变型，增加了切入45°角螺齿的通道。这些顶部切槽通道相对于心轴螺齿的角度范围约为45-135°，更个别地约为75-105°，并且根据本发明的一些方面，顶部切槽通道的角度可约为90°。这些通道的数目和深度也可以改变，并且可通过下面更简单的方式限定：[(切入心轴螺齿的总通道面积/心轴螺齿的总面积)×100％]。这个值的范围约为10-90％，更个别地约为40-60％，并且在本发明的一些实施例中这个值可约为50％。具有双横向心轴28的行星辊式挤压机可以从Rust-Mitschke-Entex公司购得。通过调整全螺齿30和开式或双横向心轴28的数目，就能控制物料穿过行星辊式挤压机的速度以及由此对物料进行素炼的量。
根据筒体的直径和工艺设计，传统的行星辊式挤压机含有至少三个并且可包含多达24个的心轴。当然，本领域的技术人员能认识到，根据挤压机的具体大小和构造，可以采用更多数目的行星心轴。在本发明的一个实施例中，采用的行星辊式挤压机10具有一个带6个心轴28、30的70mm直径的筒体。根据本发明的一些方面，双横向心轴28占行星辊式挤压机10中行星心轴28、30数目的20％以上，更个别地超过50％。图6示出根据本发明一个具体实施例的行星式挤压机横截面，该挤压机包括四个双横向行星心轴28和两个全螺齿心轴30。
主轴26的旋转使得行星心轴28、30也旋转运动，这是由于主轴26的螺旋齿轮装置和行星心轴28、30的螺旋齿轮装置相互作用的结果。
行星心轴28、30还与筒体段24的内齿轮装置啮合。主轴26、行星心轴28、30以及筒体段24的螺旋齿轮装置朝排出口34的方向传输待混合的原料。
本文所用的术语“第二原料”指的是引入行星辊式挤压机10混和段14的原料或溶剂。第二液体材料，比如液体弹性体、熔融树脂、油类、溶剂等可以通过定量环22组件经由喷嘴(未示出)引入混合段14。如图3所示，定量环22包括便于液体计量添加到混合段14的径向延伸孔23。根据本发明的一个实施例，该工序包括经由定量环22将溶剂供给进入行星辊式挤压机10的混和段14。
第二固体原料可通过侧面进料器36或双螺杆定量装置38添加到混和段14。双螺杆定量装置38通常布置为垂直于混和段14的轴线，并且通常位于直接与定量环22a相邻的混和段的开始处附近。双螺杆定量装置38可用来将固体组分(比如热塑性弹性体、树脂、补充剂、活化剂、抗降解剂、交联剂等)导入到各个辊筒段20。
本发明的另一实施例涉及将自粘性组合物涂覆到片状材料上，这里片状材料的涂覆可以利用多种涂覆技术中的任何一种进行，这些涂覆技术包括，但不限于槽模涂覆、辊-辊(roll-over-roll)涂覆，反向辊和刀-辊(knife-over-roll)涂覆。根据本发明的一些实施例，利用槽模敷料器装置将粘性组合物涂敷到片状材料上。将粘性组合物涂敷到片状材料特别有用的方法包括利用旋转唇形模或固定唇形接触模的槽模涂覆。一个可以采用的具体槽模装置是旋转唇形模，其心轴拖带模唇。这种模具的一个例子可从SIMPLAS公司购得，并在图4中示出。旋转唇形模40包括用于接收来自挤压机10的粘性组合物进口42。如图5所示，粘性组合物连续地从挤压机10输送到旋转唇形模敷料器40，以便通过槽44涂敷到片状材料上。旋转唇形模敷料器40在模唇部后缘还包括改进所涂胶粘剂涂覆性能的旋转心轴46。旋转唇形模敷料器40上的调节螺栓48可使操作人员容易地调节唇部开度和控制粘性涂层厚度。
根据本发明的另一个方面，自粘性组合物可以交联。更准确地说，涂覆的粘性组合物可以借助于电子束或通过电离辐射的UV(紫外线)射线，进行交联，例如像电子束可使产生的自粘胶带变得抗剪切和热稳定。UV射线同样也可用于交联，在这种情况下，适当的UV促进剂，例如像UCB的Ebecryl 140，必须添加到自粘性组合物中。也可以采用化学和/或热诱导的交联。
非热塑性弹性体可从天然橡胶或合成橡胶或者天然橡胶和/或合成橡胶任何所需混合物的组别中选择，可以从天然橡胶或基本上所有适用等级的橡胶中选择，例如像绉胶、RSS(皱纹烟胶)、ADS(风干橡胶片)、TSR(薄胶片)、SIR(硅橡胶)10、SIR 5L或CV等级，这取决于所需纯度和粘性水平，并且也可以从以下组别中选择合成橡胶或橡胶：无规共聚的丁苯橡胶(SBR)、聚丁橡胶(BR)、合成聚异戊二烯橡胶(IR)、丁基橡胶(IIR)、聚异丁烯橡胶、卤代丁基橡胶(XIIR)、丙烯酸盐橡胶(ACM)、乙烯乙酸乙烯酯共聚物(EVA)和聚氨酯和/或其混合物。
根据总非热塑性弹性体含量计算，可将重量分数1至100％(按重量计)的热塑性弹性体添加到非热塑性弹性体中。这里特别提及的是高度兼容的苯乙烯-异戊二烯-苯乙烯(SIS)、苯乙烯-丁二烯-苯乙烯(SBS)、苯乙烯-异戊二烯-丁二烯-苯乙烯(SIBS)等级以及SEBS和SEPS，和其任何组合作为典型物。
可以采用的增粘树脂都毫无例外地是所有能在配方中起到增粘剂作用的增粘树脂。根据弹性体计算，增粘树脂在粘性组合物中的重量分数可为40％至200％。可以提及的典型物包括松香，其歧化、氢化、聚合和酯化的衍生物以及盐类；脂肪族和芳烃树脂、萜烯树脂和萜烯-酚醛树酯。典型的树脂包括部分或完全氢化的木材、树胶或妥尔油松香，酯化的木材，树胶或妥尔油松香，α和β蒎烯树脂，和聚萜烯树脂。更准确地说，本文所用的树脂包括C5烃类树脂、C9烃类树脂及其混合物。也可使用香豆酮-茚树脂和α-甲基苯乙烯树脂。这些树脂可以固态和熔融态导入。可以使用这些和其它树脂任何所需的组合，以便根据需要调整生成的粘性组合物。特别可参考Donatas Satas著的“压敏胶粘剂技术手册”(van Nostrand，1989)中的技术水平描述。
典型的补充剂包括粘土、碳酸钙、滑石和氢氧化铝。典型的活化剂包括氧化锌、氯化锌、氯化镁和氧化镁。典型的抗降解剂包括抗氧剂(AO)、紫外线吸收剂(UVA)和紫外线稳定剂(UVS)。典型的遮光剂和着色剂包括，但不限于二氧化钛和本领域技术人员所知的其它各种金属颜料。
典型的溶剂是非极性的芳香族和脂肪族化合物，比如丙酮、甲苯、己烷、庚烷及其混合物。当需要高度起泡的胶粘剂时，可以增大胶粘剂中溶剂的含量。这方面公开的内容解决了普通热熔胶粘剂通常遇到的问题，即由于挤出的胶粘剂表面密度较高和平滑不能延伸造成成品胶粘剂低的粘性与附着力比所带来的问题。溶剂在配方中时以粘性组合物重量计可采用大约70％以下的任何量，更个别地大约50％以下。典型的液体弹性体是低分子量的天然橡胶和低分子量的合成聚异戊二烯和聚丁烯橡胶。典型的油类可以是石蜡的、异链烷烃的、环烷的、芳香族的或聚芳香族(polyaromatic)的。发泡剂的例子包括Cellogen发泡剂和气体。
可以使用的增塑剂是胶带技术中已知的所有增塑物质。有用的增塑剂例子包括，但不限于石蜡和环烷油类、(功能化的)齐聚物，比如低聚丁二烯(oligobutadiene)和低聚异戊二烯(oligoisoprene)、液体腈橡胶、液体萜烯树脂、动物和植物油以及脂肪、邻苯二酸盐、和功能化的丙烯酸盐。
简而言之，新发明/方法的某些实施例的一些优点包括：1)非热塑性弹性体素炼有效果、起作用和高效，2)将各种固体原料引入混和段，3)将溶剂引入混和段，和4)使用槽模涂覆技术，获得涂覆胶粘剂的片状材料有着会聚面(converged panel)附着力和快速粘附性能的独特平衡。
由于用单螺杆迫使弹性体从定量环和主轴之间的进料段进入混和段，在这里，强烈地混合及随后素炼，因而实现了非热塑性弹性体有效果的素炼。通过使用双横向行星心轴进一步增强了素炼的程度。另一个影响素炼量的因素是止动环的内径。通过使止动环或定量环与心轴之间的间隙变窄，就能进行更多的素炼。非热塑性弹性体的素炼使弹性体与其它固体和液体材料变得更有效的混合，使成品胶粘剂产生更大的粘性与附着力比潜力，而且产生的成品胶粘剂具有且不限于经由多辊敷料器装置(压延机)所涂覆的较低粘度。与购买多辊涂覆装置不同，它提供了采用更流行或现有涂覆设备的机会。
根据本发明的一个方面，弹性体这样素炼，以使用GPC测量时Mw减小至小于1,000,000。在本发明的其它方面，弹性体可素炼使得Mw减少超过约50％，更个别地超过约80％，相对于弹性体的初始Mw而言。初始分子量指的是非热塑性弹性体在其引入行星辊式挤压机时的分子量。这样，与未加工的弹性体分子量相比，由于弹性体进行了预加工，故初始分子量可能已经减少。因此，本文所指的分子量减少是基于通过行星辊式挤压机加工获得的分子量的减少。本文所述的分子量减少率用公式I计算：
(I)减少率，％＝(Mw(初始)-Mw(最终))/Mw(初始)×100
将各种固体原料引入混和段具有几个优点。首先，所有的固体原料不必同时引入行星辊式挤压机的进料段，也就是这些物料可在混和段的一个或多个辊筒段内进行配料。这样使得弹性体在加入固体原料之前有更多的时间进行素炼，并且提高了行星辊式挤压机的混合效率。其次，固体树脂与熔融树脂不同，可以引入混和段。与熔融树脂相比，固体树脂的粘度更接近类似弹性体。因此，固体树脂的加入(与液体树脂对比)进一步提高了混合效率，而熔融树脂往往会起到润滑剂的作用，并且阻碍混合效率。另外，固体树脂具有使其能起到散热器作用的比热，也就是从工序中散热，从而将混合过程中的熔化温度降至最低程度。相反，熔融树脂升高了混合过程中的熔化温度。
将溶剂引入混和段具有几个优点。首先，少量(例如通常以重量计有可能使用10至20％，不过也可达到50％)通过几个定量环引到胶粘剂的溶剂提高了混合效率，即保持了均匀性，同时显著降低了成品胶粘剂的粘度。溶剂迅速被粘性组合物吸收，并且溶剂的混入将产生的均匀胶粘剂的粘度降低至这种程度，即其在片状材料上的涂敷不限于多辊敷料器装置(压延机)。而是这时，较低粘度的胶粘剂可由槽模、反向辊、辊-辊、刀-辊或其它传统的胶粘剂涂敷技术(包括使用多辊敷料器)涂敷到片状材料。随后将溶剂从已涂敷到片状材料的胶粘剂中析出就能对粘膜中许多粘性表面几何外形，即发泡程度起作用。其后，可进一步控制粘膜的工作性质，即除了弹性体素炼程度和配方外。
使用槽模将胶粘剂涂覆到片状材料上具有优于多辊敷料器装置(压延机)的特殊优点。在使用多辊敷料器装置(压延机)时，片状胶粘剂涂覆速度通常限于每分钟300米。然而，使用槽模涂覆技术，尤其是在和较低粘度高固体的胶粘剂(例如80-90％)结合使用时，与较高粘度100％固体的胶粘剂不同，具有特殊的影响，因为涂敷速度很容易地达到每分钟500米或更高。
本发明的工艺使能生产高性能的自粘性组合物，特别是结合下游的涂覆和交联装置，使能生产高性能的自粘胶带，并伴有特殊的成本优势。
在第一加工步骤中，包括弹性体和制造自粘性组合物所需的已知辅料(adjuvant)(比如补充剂、抗氧化剂、活化剂、着色剂、老化抑制剂、增塑剂和增粘树脂)的组合物在行星辊式挤压机中制造，该组合物具有低于150℃的最终温度，通常低于130℃，并且更个别地介于约25℃和100℃之间。组合物在行星辊式挤压机中的总停留时间通常不超过约三分钟。
根据本发明的一些方面，将来自挤压机的粘性组分涂敷到片状材料上。这可以利用槽模敷料器装置，特别是利用与图4所示类似的旋转唇形槽模敷料器装置，以特别有效且有利的方式做到。
根据本发明的另一方面，自粘性组合物可以利用电子束或UV射线进行交联，以构成具有所需性能的自粘胶带。为了进一步改进性能，或在电子束(EBC)-敏感载体的情况下，同样可以借助于热活化交联剂在温度的作用下进行交联。对为此目的所需的压敏胶粘剂组合物加热可借助于已知技术完成，尤其是借助于高温管道，否则借助于红外线灯，或者借助于高频交变磁场，其例子有高频(HF)波、超高频(UHF)波或微波。
压敏胶粘剂组合物的交联还可借助于电离辐射与热活化化学交联剂结合进行。其结果可以是高度抗剪切的压敏自粘性组合物。电子束(EB)固化将胶粘剂凝固，使得它在具有残留的可用于最终涂敷使用的潜热活化固化剂时可以转化。
为了热诱导和/或化学交联，在本发明的工艺中可以使用所有已知的热活化和/或化学交联剂，比如加速硫或硫给予体系统、异氰酸盐系统、活性三聚氰酰胺树脂、具有相应活化剂的甲醛树脂和(任选卤代的)苯酚-甲醛树脂和/或活性酚醛树脂或二异氰酸盐(diisocyanate)交联系统、环氧化聚酯树脂和丙烯酸盐树脂及其组合。
交联剂优选在50℃以上的温度活化，特别在100℃到160℃的温度，并且根据一些实施例，在110℃到140℃的温度。交联剂的热激发也可通过IR(红外线)射线或高能交流电场完成。一些交联剂在固化之后可保留在组合物中，因而，在最终涂敷使用过程中可用于活化。
本发明概念所涵盖的还有利用压敏胶粘剂组合物通过将自粘性组合物涂敷到片状材料至少一面来制造自粘胶带。根据粘性胶带的预计用途，适用于根据本发明加工和制造的自粘性组合物的片状载体物料都是已知的载体，其涂敷面具有或没有进行适当的化学或物理表面预处理，而反面进行抗粘性物理处理或涂覆。例如，可以提及皱纹纸或不皱纹纸、聚乙烯、聚丙烯和单轴向或双轴向聚丙烯薄膜、聚酯、PVC和其它薄膜，由聚乙烯和聚氨酯制成的泡沫片状材料，例如织物、针织物和非织物。最后，片状材料可以是在两面具有抗粘涂层(比如防粘(release)纸或防粘薄膜)的材料。
自粘性组合物在片状材料上的厚度可以在10μm和2000μm之间，优选在15μm和150μm之间。最后，自粘性组合物可以800μm至1200μm的厚度涂敷到防粘纸上。这类粘性组合物层，特别在交联之后，可不同地用作无衬里(backing-less)的双面自粘胶带。
以下例子示出本发明的多个方面，但不限于此。可以理解，在本领域技术人员的技能之内，在不偏离本发明精神和范围的前提下可对本发明进行另外的修改。
示例
例1
                               磨碎的天然橡胶     磨碎的橡胶胶粘剂
橡胶(Kg/hr)                    不详               17.1
树脂(Kg/hr)                    不详               22.2
TiO2+抗氧化剂(Kg/hr)           不详               0.7
螺杆速度(rpm)                  不详               70
筒体1和2之间的胶粘剂温度       不详               72℃
筒体2和3之间的胶粘剂温度       不详               52℃
胶粘剂出口温度                 不详               86℃
挤压机停留时间(s)                                 90
胶粘剂均匀性                                      无凝胶
Mw(GPC)                        4,136,110          802,748
Mw下降率                                          80.6％
Mw(ThFFF)                      3,724,000          691,000
Mw下降率                                          81.5％
曾用具有三个筒体的行星辊式挤压机(PRE)制造出标准的纸板密封胶粘剂，加入有100phr天然橡胶、130phr C5树脂、2phr TiO2和2phr抗氧化剂。用于这种胶粘剂中的橡胶是SIR5L，磨碎为8mm的平均粒度，采用滑石作为抗凝结剂。C5树脂以片状加入，引入的抗氧化剂为粉末。胶粘剂原料全部加入70mm PRE的进料喉部。原料随后在三个400mm圆筒段中混合之后混入胶粘剂中，每个圆筒段含有两个正常和四个双横向以70rpm转动的混合心轴。成品胶粘剂经测定是完全均匀的(无凝胶)。其后胶粘剂的分子量分析由凝胶渗透色谱法(GPC)和热场流动分析法(ThFFF)完成。分子量分析显示，天然橡胶的分子量降低了大约80％。
例2
                                     磨碎的橡胶胶粘剂
橡胶(Kg/hr)                          17.1
树脂(Kg/hr)                           22.2
TiO2，抗氧化剂(Kg/hr)                 0.7
溶剂(甲苯)                            12.0
螺杆速度(rpm)                         65
筒体1和2之间的胶粘剂温度              62℃
筒体2和3之间的胶粘剂温度              57℃
胶粘剂出口温度                        42℃
挤压机停留时间(s)                     90
胶粘剂均匀性                          无凝胶
曾用具有三个筒体的行星辊式挤压机制造出标准的纸板密封胶粘剂，加入有100phr天然橡胶、130phr C5树脂、2phr TiO2和2phr抗氧化剂。用于这种胶粘剂中的橡胶是SIR5L，磨碎为8mm的平均粒度，采用滑石作为抗凝结剂。C5树脂以片状加入，引入的抗氧化剂为粉末。胶粘剂原料全部加入70mm PRE的进料喉部。原料随后在最初三个400mm圆筒段中混合之后混入胶粘剂中，每个圆筒段含有两个正常和四个双横向以65rpm转动的混合心轴。全部补充溶剂通过插入定量坏的喷射阀加入。成品胶粘剂经测定完全成溶剂化物而且均匀(无凝胶)。
例3
                               制成粒状的天然橡胶       制成粒状的橡胶胶粘剂
橡胶和抗氧化剂(Kg/hr)           不详                    14.08
树脂(Kg/hr)                     不详                    15.88
填料、ZnO、TiO2(Kg/hr)          不详                    7.93
螺杆速度(rpm)                   不详                    70
筒体1和2之间的胶粘剂温度         不详                    59℃
筒体2和3之间的胶粘剂温度         不详                    53℃
胶粘剂出口温度                   不详                    76℃
挤压机停留时间(s)                                        90
胶粘剂均匀性                                             无凝胶
Mw(GPC)         1,026,671         489,279
Mw下降率                          52.3％
Mw(ThFFF)       666,000           310,000
Mw下降率                          53.5％
曾用具有三个筒体的行星辊式挤压机制造出标准的掩蔽用纸带(masking tape)胶粘剂，加入有100phr天然橡胶、115phr C5树脂、50phr高岭粘土、5phr ZnO、2.5phr TiO2和2phr抗氧化剂。用于这种胶粘剂中的橡胶是SIR5L，在班伯里混炼机中预素炼并与2phr抗氧化剂混炼，且随后在湿式造粒机(underwater pelletizer)中进行加工，以产生8mm的粒状制品，采用滑石作为抗凝结剂。C5树脂以片状加入，引入的ZnO和TiO2为粉末。胶粘剂原料全部加入70mm PRE的进料喉部。原料随后在三个400mm圆筒段中混合之后混入胶粘剂中，每个圆筒段含有两个正常和四个双横向以70rpm转动的混合心轴。成品胶粘剂经测定是完全均匀的(无凝胶)。其后胶粘剂的分子量分析由凝胶渗透色谱法(GPC)和热场流动分析法(ThFFF)完成。分子量分析显示，天然橡胶的分子量降低了大约50％。
例4
                                       制成粒状的橡胶胶粘剂
橡胶和抗氧化剂(Kg/hr)                   14.08
树脂(Kg/hr)                             15.88
填料、ZnO、TiO2(Kg/hr)                  7.93
溶剂-甲苯(Kg/hr)                        40.0
螺杆速度(rpm)                           144
筒体1和2之间的胶粘剂温度                64℃
筒体2和3之间的胶粘剂温度                29℃
胶粘剂出口温度                          29℃
挤压机停留时间(s)                       120
胶粘剂均匀性                            无凝胶
曾用具有三个筒体的行星辊式挤压机制造出标准的掩蔽用纸带胶粘剂，加入有100phr天然橡胶、115phr C5树脂、50phr高岭粘土、5phr ZnO、2.5phr TiO2和2phr抗氧化剂。用于这种胶粘剂中的橡胶是SIR5L，在班伯里混炼机中预素炼并与2phr抗氧化剂混炼，且随后在湿式造粒机中进行加工，以产生8mm的粒状制品，采用滑石作为抗凝结剂。C5树脂以片状加入，引入的ZnO和TiO2为粉末。胶粘剂原料全部加入70mm PRE的进料喉部。原料随后在最初三个400mm圆筒段中混合之后混入胶粘剂中，每个圆筒段含有两个正常和四个双横向以144rpm转动的混合心轴。溶剂通过插入定量环的喷射阀加入，5kg/hr加入位于圆筒1和2之间的定量环，35kg/hr加入位于圆筒2和3之间的定量环中。成品胶粘剂经测定完全成溶剂化物而且均匀(无凝胶)。
例5
                                     磨碎的橡胶胶粘剂
橡胶和抗氧化剂(Kg/hr)                 14.76
树脂-进料喉部(Kg/hr)                  8.00
树脂-侧面进料器(Kg/hr)                8.64
填料、ZnO、TiO2(Kg/hr)                8.32
溶剂-甲苯-2/3(Kg/hr)                  11.0
溶剂-甲苯-3/4(Kg/hr)                  29.0
螺杆速度(rpm)                         141
筒体1和2之间的胶粘剂温度               120℃
筒体2和3之间的胶粘剂温度               60℃
筒体3和4之间的胶粘剂温度               33℃
胶粘剂出口温度                         21℃
挤压机停留时间(s)                      73
胶粘剂均匀性                           无凝胶
曾用具有四个筒体的行星辊式挤压机制造出标准的掩蔽用纸带胶粘剂，加入有100phr天然橡胶、115phr C5树脂、50phr高岭粘土、5phr ZnO、2.5phr TiO2和2phr抗氧化剂。用于这种胶粘剂中的橡胶是SIR10，磨碎为8mm的平均粒度，采用滑石作为抗凝结剂。一部分C5树脂以片状加入70mm PRE的进料喉部，同时加入ZnO和TiO2粉末。原料随后在最初四个400mm圆筒段中混合，每个圆筒段含有两个正常和四个双横向以141rpm转动的混合心轴。剩余的片状树脂由紧邻位于第一定量环上游的侧面进料器加入，并且随后在第二圆筒段中进行混合。溶剂由插入定量环的喷射阀加入，11kg/hr加入位于圆筒2和3之间的定量环，29kg/hr加入位于圆筒3和4之间的定量环中。成品胶粘剂经测定完全成溶剂化物而且均匀(无凝胶)。
已经描述了本发明的各个方面和实施例及其几个优点，本领域的普通技术人员将认识到，在所附权利要求的精神和范围内，容许对本发明作各种改进、替换和修改。

Claims (36)

1.一种制备胶粘剂的工艺，该工艺包括步骤：
a.)将包括非热塑性弹性体的初始原料引入行星辊式挤压机的进料段；
b.)将初始原料从进料段传输到行星辊式挤压机的混和段；
c.)在混和段里使初始原料与固体增粘树脂混合，其中混和段包括有被多个行星心轴所包围并与之相啮合的主轴，其中至少行星心轴之一是包括多个顶部切槽螺齿的双横向混合心轴；
d.)制出均匀的粘性组合物；和
e.)将粘性组合物涂敷到片状材料上。
2.如权利要求1所述的工艺，其中混和段包括3至24个行星心轴。
3.如权利要求1所述的工艺，其中混和段还包括具有全螺齿的行星心轴。
4.如权利要求3所述的工艺，其中双横向混合心轴占混合段中行星心轴总数的20％以上。
5.如权利要求4所述的工艺，其中混和段包括两倍于具有全螺齿的心轴数量的双横向心轴。
6.如权利要求1所述的工艺，还包括将第二原料加入混和段。
7.如权利要求6所述的工艺，其中第二原料包括选自由热塑性弹性体、补充剂、活化剂、交联剂、着色剂及其混合物组成的组别中的固体原料。
8.如权利要求6所述的工艺，其中第二原料包括选自由液态弹性体、熔融树脂、油类、溶剂及其混合物组成的组别中的液体原料。
9.如权利要求8所述的工艺，其中溶剂选自由丙酮、甲苯、己烷、庚烷及其混合物组成的组别。
10.如权利要求1所述的工艺，其中混和段包括多个辊筒段。
11.如权利要求10所述的工艺，其中每个辊筒段包括有双横向心轴。
12.如权利要求11所述的工艺，其中初始原料包括天然橡胶和增粘树脂。
13.如权利要求11所述的工艺，其中初始原料还包括选自由氧化锌、氧化镁及其混合物组成的组别中的活化剂以及选自由粘土、碳酸钙、滑石、氢氧化铝及其混合物组成的组别中的补充剂。
14.如权利要求1所述的工艺，其中弹性体这样素炼以使Mw在用GPC法测量时减少至小于1,000,000。
15.如权利要求1所述的工艺，其中非热塑性弹性体选自由天然橡胶、合成聚异戊二烯、丁苯橡胶、丁基橡胶、聚异丁烯橡胶及其混合物组成的组别。
16.如权利要求1所述的工艺，其中将粘性组合物涂敷到片状材料的步骤包括选自由槽模涂覆、反向辊、辊-辊涂覆和刀-辊涂覆组成的组别中的涂覆工艺。
17.如权利要求1所述的工艺，其中涂覆工艺包括用旋转唇形模或固定唇形接触模的槽模涂覆。
18.如权利要求1所述的工艺，还包括：
f.)交联粘性组合物。
19.如权利要求18所述的工艺，其中步骤f包括使用选自由电子束(EB)交联、紫外线(UV)交联、热和/或化学交联及其组合组成的组别中的工艺交联粘性组合物。
20.一种制造粘性组合物的工艺，包括：
a.)将包括非热塑性弹性体和增粘树脂的粘性组合物初始原料连续地计量进入行星辊式挤压机；
b.)在行星辊式挤压机的混和段里连续地使初始原料与固体增粘树脂混合，以形成均匀的粘性组合物，其中混和段包括有被多个行星心轴所包围并与之相啮合的主轴，其中至少行星心轴之一是包括多个顶部切槽螺齿的双横向混合心轴；和
c.)将均匀的粘性组合物连续地从挤压机中排出。
21.如权利要求20所述的工艺，其中非热塑性弹性体选自由天然橡胶、合成聚异戊二烯、丁苯橡胶、丁基橡胶、聚异丁烯橡胶及其混合物组成的组别。
22.如权利要求21所述的工艺，其中非热塑性弹性体包括预素炼的天然橡胶。
23.如权利要求20所述的工艺，其中混和段包括多个辊筒段。
24.如权利要求23所述的工艺，其中每个辊筒段包括至少一个双横向混合心轴。
25.如权利要求20所述的工艺，还包括在混和段中向原料加入溶剂。
26.如权利要求20所述的工艺，还包括：
d.)将粘性组合物涂敷到片状材料上。
27.如权利要求26所述的工艺，其中用槽模涂料器、反向辊、辊-辊涂覆和刀-辊涂覆将粘性组合物涂敷到片状材料上。
28.如权利要求26所述的工艺，其中片状材料选自由纸、聚乙烯、聚丙烯、聚酯、聚氯乙烯及其混合物组成的组别。
29.如权利要求28所述的工艺，还包括交联粘性组合物。
30.如权利要求20所述的工艺，还包括将第二原料加入到混和段。
31.如权利要求30所述的工艺，其中第二原料包括固体材料。
32.如权利要求31所述的工艺，其中固体材料选自由热塑性弹性体、树脂、补充剂、活化剂、抗降解剂、交联剂及其混合物组成的组别。
33.如权利要求31所述的工艺，其中混和段还包括双螺杆定量装置，并且固体材料由该双螺杆定量装置加入到混和段。
34.一种制备胶粘剂的工艺，该工艺包括步骤：
a.)将包括具有初始分子量(Mw(初始))的非热塑性弹性体的初始原料引入行星辊式挤压机的进料段；
b.)将初始原料从进料段传输到行星辊式挤压机的混和段；
c.)在混和段里使初始原料与固体增粘树脂混合，其中混和段包括有被多个行星心轴所包围并与之相啮合的主轴；
d.)制出均匀的粘性组合物，其中非热塑性弹性体(i)具有小于1,000,000的最终分子量(Mw(最终))或者(ii)根据公式I计算显示Mw的减少率(％)超过大约50％：
(I)减少率％＝(Mw(初始)-Mw(最终))/Mw(初始)×100；和
e.)将粘性组合物涂敷到片状材料上。
35.如权利要求34所述的工艺，还包括将第二原料加入混和段。
36.如权利要求35所述的工艺，其中第二原料包括溶剂。
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