CN107073767B - 用于制造三维泡沫制品的方法 - Google Patents

用于制造三维泡沫制品的方法 Download PDF

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CN107073767B
CN107073767B CN201580036997.9A CN201580036997A CN107073767B CN 107073767 B CN107073767 B CN 107073767B CN 201580036997 A CN201580036997 A CN 201580036997A CN 107073767 B CN107073767 B CN 107073767B
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保罗·雅各布斯
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Abstract

本发明公开了一种用于制造非均匀形状的三维泡沫制品的方法，该方法采用了两阶段氮压力釜方法和在至少一个尺寸上具有非均匀横截面的预制件。

Description

用于制造三维泡沫制品的方法
发明领域
本发明涉及用于制造非均匀形状的三维泡沫制品的方法，并且尤其是使用氮压力釜方法的方法。
发明背景
氮压力釜方法已经用于商业上制造聚合物泡沫许多年，并且在一些细节上描述于专利US 3,640,915和GB 899,389，以及书籍如由S.T.Lee和D.Scholz编写的《聚合物泡沫(Polymeric Foams)》(CRC出版社，2009年)和由D.Eaves编写的《聚合物泡沫手册(Handbookof Polymer Foams)》(Rapra Technology Limited，2004年)。所述工艺通常包括三个阶段；在第一阶段中，制造固体聚合物制品，在第二阶段中，在高压下并且在高温下将气体吸收至聚合物中，并且在最后阶段中，使制品膨胀以制造泡沫。
在现有技术水平下，挤出通常用于制造第一阶段的固体聚合物制品，因为这是制造扁平片材的成本有效的方法，其相对容易操控并且允许发泡工艺的随后阶段所需的在压力釜中的高效加载。然而，尽管挤出工艺确实制造了可以容易且有效地加载至压力釜中的固体聚合物制品，其将最终产品的形式限制为均匀厚度的基本上二维的矩形片材，并且尽管产品的片材形式可以适用于许多应用，越来越清楚的是，对于许多高体积应用如在跑步鞋中使用的中底(midsole)来说，变化厚度的近终形(near-net-shape)制品将会是高度理想的。
在US2003/0046832；US6776939；US6787079；US7052634；US7464428；US8906280；GB2014153A和US2014/0259801中公开了多种采用预制件的方法。在US6993858；US7146751和US6439536中公开了其他方法。
用于制造三维聚合物泡沫制品的其他方法也是本领域技术人员已知的，然而，这些通常没有制造均匀密度或各向同性泡孔结构(cell structure)的制品。例如，珠泡沫方法通常导致其中存在发泡部分的厚度变化的密度变化，并且即使泡沫的初始泡孔结构是各向同性的，热成形方法也通常导致形成各向异性的泡孔结构。
发明概述
已经发现，通过将在氮压力釜方法的第一阶段中使用的通常的片材挤出方法替换为形成氮压力釜方法的第二和第三阶段所需的固体聚合物制品的另一种方法，可以制造近终形发泡制品，或者在一些实例中成品泡沫制品。对于形成固体聚合物制品的方法来说，尽管预期了其他方法，如压缩成型、机械加工或增材制造(即3D打印)，但是已经确定将注塑成型确定为用于高体积应用的优选方法，尤其是对于不能证明昂贵的工具加工的成本的合理性的小规模制造运营来说。
因此，在一个方面中，本发明提供一种用于制造非均匀形状的三维泡沫制品的方法，所述方法包括下列步骤：
(a)在压力容器中提供包含聚合物的预制件，
(b)使所述预制件在高于大气压的压力下经历至少一种惰性气体，以迫使气体进入所述预制件中，
(c)将所述预制件的温度升高至其软化点以上，其中步骤(b)和(c)可以以任意顺序或同时进行，
(d)将所述压力降低至高于大气压但是低于步骤(b)的所述压力的压力，并且之后将所述预制件冷却至低于其软化点，以得到部分膨胀的制品，
(e)将所述制品转移至第二容器并且在惰性气体或空气的压力下将其加热至高于其软化点的温度，和
(f)在将所述温度维持在等于或高于所述聚合物的软化点的同时降低所述压力，以使所述部分膨胀的制品膨胀而形成发泡制品，
其中所述聚合物预制件在至少一个尺寸(优选两个、最优选三个尺寸)上的横截面是非均匀的。
所得的发泡制品的泡孔结构优选为各向同性的。
备选地，本发明提供一种用于制造非均匀形状的三维泡沫制品的方法，所述方法包括下列步骤：(a)制备固体聚合物预制件，(b)使所述固体聚合物预制件在高于大气压的压力下经历至少一种惰性气体，以迫使气体进入所述聚合物预制件中，(c)将所述聚合物预制件的温度升高至其软化点以上，其中步骤(b)和(c)可以以任意顺序或同时进行，(d)在将所述温度维持在等于或高于所述软化点的同时降低所述压力，以使所述聚合物预制件膨胀为发泡制品，其中优选地，所述聚合物预制件在至少一个尺寸(优选两个、最优选三个尺寸)上的横截面是非均匀的。
本发明方法与现有技术方法之间的关键区别在于，使预制件预成形以制造近终形的成品产品。这允许更容易地并且以最小废料制造具有不同横截面的更复杂的泡沫形状。常规形状的扁平片材需要大量的二次操作以实现复杂的形状，并且产生通常大量的废料，尤其是如果部件是不规则形状的或具有切口的话。
可以降低由步骤(d)得到的部分膨胀的聚合物预制件的温度以延缓气体从聚合物预制件中的损耗。例如，可以将充气的预制件转移至冰箱以防止气体损耗，从而如果需要的话，使得充气和膨胀之间的时间更长。这是可以任选在所述方法的步骤(d)和(e)之间进行的额外步骤。在制造的上下文中，充气和膨胀步骤的分开非常有帮助的，因为其使得膨胀阶段延迟，使膨胀容器的获得或者甚至充气预制件向在不同位置的膨胀容器的输送待定。因此，可以将步骤(d)的部分膨胀的制品在转移至步骤(e)的第二容器之前储存一段时间(优选至少4小时，更优选至少12小时，最优选至少24小时)。
所述方法可以是间歇方法。
优选为将预制件的聚合物交联，并且聚合物组成可以包含助剂以改变所述聚合物的交联行为。如果将聚合物交联，则其可以通过用电子束或用γ射线对其进行辐射来交联。辐射剂量优选为5至200kGy。
预制件的聚合物可以包含一种或多种热塑性树脂，并且如果是这样的话，则热塑性树脂中的一种或多种可以是热塑性弹性体(TPE)。还更优选地，热塑性弹性体中的一种或多种可以是聚醚嵌段酰胺(PEBA)和/或热塑性树脂中的一种或多种可以是热塑性聚氨酯(TPU)。
优选地，预制件的聚合物基本不含成核剂，然而，其可以被染色或者包含其他本领域技术人员已知的添加剂、改性剂或增强材料，包括功能性添加剂如导电添加剂、抗微生物剂、阻燃剂和防烟剂。
可以将聚合物预制件注塑成型。如果是这样的话，则可以使用重叠注塑(overmoulding)、嵌入成型、双喷射或多喷射注入或共注入方法将聚合物预制件注塑成型。
备选地，可以将聚合物预制件压缩成型。
在另外的备选方案中，可以使用增材制造(additive manufacturing)或3D打印方法制造聚合物预制件。
最后，可以将聚合物预制件挤出或共挤出。
聚合物预制件可以是2.5D形状或3D形状。
发泡制品也可以是2.5D形状或3D形状。如果是这样的话，则还可以将发泡制品热成形以产生第二3D形状。在这种情况下，发泡制品可以是鞋的中底。
优选的是，发泡制品的具有相同聚合物组成的区域是基本上均匀的。还优选的是，发泡制品的具有相同聚合物组成的区域的热和机械性能是各向同性的。
发泡制品优选具有小于300kg/m3的密度。
有利地，步骤(b)中的压力是20至1000巴，并且还更优选20至800巴。特别有利的是，在步骤(b)期间维持恒定压力从而将已知量的气体吸收至预制件中，从而更准确地控制成品制品的密度。在步骤(d)的最后仅将预制件部分膨胀也是特别有利的，因为在该步骤最后压力的释放将会引起显著的绝热冷却，这使得难以控制膨胀过程，因为在特定温度下，聚合物可能会变得过冷而适当膨胀并且部件也可能会变得扭曲。另外，使用高压压力釜将泡沫充分膨胀是非常低效的，因为由每个循环产生的泡沫的体积大大低于可以通过使用用于两阶段方法中的步骤(e)和(f)的较大但是较低压力的第二容器产生的泡沫的体积。
步骤(e)中的压力优选为5至200巴，并且还更优选5至40巴。
如果将预制件的聚合物交联，则步骤(c)中的温度优选为高于软化点5至135℃。如果将预制件的聚合物交联，则步骤(e)和(f)中的温度也应当优选为高于聚合物的软化点5至135℃。
注塑成型是特别有利的，尤其是在使用高价值聚合物的情况下，因为其允许以最少的废料制造大量的部件。其还提供了尺寸准确的部件并且允许实现高水平的细节，例如，薄的截面和有纹理的表面。还预期了重叠注塑和多次喷射注入成型，其中不同的成型区域由具有不同性能的不同材料组成。在这样的实例中，将会需要聚合物或化合物以及加工参数的仔细选择，以及模具的设计，从而防止由差异发泡行为导致的最终发泡部件的扭曲。这样的差异发泡行为可能由诸如不同材料的气体吸收特性、流变行为和热膨胀行为之类的因素导致。
优选地，固体聚合物制品是2.5D形状(即基本上在一侧上扁平并且具有波状外形轮廓)，如中底预锻模件，因为这限制了氮压力釜方法的气体吸收或膨胀阶段(二者优选在聚合物的软化点以上进行)期间制品塌落(slump)或扭曲的可能性。然后可以使用随后的压缩成型或其他本领域技术人员已知的泡沫制造工艺将近终形发泡制品成形为完全三维(3D)的成品制品。
已经发现，特别有利的是，在所述方法的气体吸收和膨胀阶段之前将聚合物预制件交联，从而实现良好的尺寸准确性和膨胀均匀性。交联的水平以及气体吸收阶段的温度和压力也可以用于影响泡沫的膨胀程度和最终物理性质，并且在任何随后的加工如热成形中可以是有益的。在预制件由不同材料的区域组成的情况下，交联可以用于控制不同区域的膨胀行为，以确保发泡部件具有所需尺寸。例如，不相似的聚合物可能需要不同的交联水平，以在所述方法的气体吸收阶段期间经历相同的温度和压力时提供相似的膨胀比。值得注意的是，在第一种情况中，对于每种聚合物来说，可以独立地确定对于任何给定的温度和压力的所需交联水平。
还预期的是，通过使用交联来控制膨胀行为，可以制造具有不同密度和不同特性(例如物理性质如硬度或回弹性)的发泡部件。通过如使用助剂的方法或者通过在使用辐射的情况下改变辐射剂量，可以来实现改变聚合物中的交联水平。在预制件由单一材料组成的情况下，通过将预制件的不同区域暴露于不同水平的辐射，例如通过预制件的掩蔽或通过辐射源的精确靶向，仍然可以实现材料的差异交联。在所有使用不相似材料或差异交联的情况中，必须注意固体聚合物预制件的设计以适应材料的膨胀比的任何差异，从而确保发泡部件具有所需尺寸和物理性质。
实施例
以下实施例仅是说明本发明的优选实施方案。
实施例1
将聚醚嵌段酰胺(PEBA)聚合物(来自Arkema的Pebax 5533)与可辐射交联添加剂混合以制备可交联PEBA材料。然后使用由Pebax 5533制造商推荐的标准注塑成型条件将可交联PEBA材料注塑成型为足球鞋底板的形式。然后使注塑成型底板经历γ射线以将PEBA材料交联。在辐射之后，注塑成型件颜色略暗，但是未显示出明显的尺寸变化。
将交联的注塑成型件放置在高压压力釜中的托盘上，并且在400巴和165℃下经历氮气气氛，直到聚合物完全被气体饱和。然后将压力降低至170巴，以使泡孔结构成核，之后将压力釜冷却至环境温度。一旦处于环境温度，就将剩余的压力释放并且从高压压力釜中移出含有气体的注塑成型件。在这个阶段，注塑成型件明显颜色较淡，并且由于成核的泡孔结构显示出4％的尺寸增加。
将部分膨胀注塑成型件放置在-40℃的冰箱中过夜以使在膨胀之前的任何气体损耗最小化。次日，使注塑成型件恢复至室温，之后放置在较低压力的压力釜中的托盘上。然后在14巴的氮的压力下将注塑成型件加热至167℃的均匀温度，之后将释放压力至大气压，使得成型件膨胀以形成发泡部件。
尽管注塑成型件的厚度变化大，但是足球鞋底板的膨胀在所有方向上是基本上均匀的。线性膨胀比率是2.35±0.15，其等于80kg/m3的最终泡沫密度。
实施例2
将聚醚嵌段酰胺(PEBA)聚合物(来自Arkema的Pebax 5533)与可辐射交联添加剂混合以制备可交联PEBA材料。然后使用由Pebax 5533制造商推荐的标准注塑成型条件将可交联PEBA材料注塑成型为左右脚的1/2.5比例跑步鞋中底预制件的形式。计算1/2.5比例预制件尺寸，得到尺寸在70kg/m3的目标密度下的膨胀中底的所需尺寸。然后使注塑成型预制件经历γ射线从而将PEBA材料交联。在辐射之后，注塑成型件颜色略暗，但是未显示出明显的尺寸变化。
将交联的注塑成型件成双地放置在高压压力釜中的托盘上，并且在270巴和165℃下经历氮气气氛，直到聚合物完全被气体饱和。然后将压力降低至150巴，以使泡孔结构成核，之后将压力釜冷却至环境温度。一旦处于环境温度，就将剩余的压力释放并且从高压压力釜中移出含有气体的成型件。在这个阶段，成型件由于成核的泡孔结构而明显颜色较淡。成型件还稍微变平并且显示出小的尺寸增加(＜2％)。
将部分膨胀成型件放置在-40℃的冰箱中以使在膨胀之前的气体损耗最小化。在膨胀之前，使注塑成型件恢复至室温，之后成双地放置在较低压力的压力釜中的托盘上。然后在14巴的氮的压力下将一双成型件加热至167℃的均匀温度，之后将释放压力至大气压，使得成型件膨胀以形成发泡中底。
跑步鞋中底的膨胀在所有方向上是基本上均匀的。线性膨胀比率是2.4±0.1，这等于73kg/m3的最终泡沫密度。
比较例
按照实施例2中描述来制备交联PEBA跑步鞋中底预制件。如前所述，在辐射之后，注塑成型件颜色略暗些，但是未显示出明显的尺寸变化。将交联的注塑成型件成双地放置在高压压力釜中的托盘上，并且在270巴和165℃下经历氮气气氛，直到聚合物完全被气体饱和。然后将压力降低至大气压，以使成型件膨胀而形成发泡中底，然后将压力釜冷却至环境温度。一旦处于环境温度，就从高压压力釜中移出含有气体的成型件。
不同于实施例2，成型件不膨胀至其完全尺寸并且变得扭曲。然而，成型件明显颜色较淡，这说明在所述方法期间已经发生了一定程度的成核和单元生长。线性膨胀比率仅为1.1±0.15，其等于700kg/m3的最终泡沫密度。
所描述的实施方案的所有任选的和优选的特征和修改以及从属的权利要求都可以用于在本文中教导的本发明的所有方面。此外，从属的权利要求的单独特征以及所描述的实施方案的所有任选的和优选的特征和修改是可以彼此组合并且互换的。
在本申请所要求优先权的英国专利申请号1409248.0中以及本申请所附摘要中的公开内容通过引用结合在本文中。

Claims (23)

1.一种用于制造非均匀形状的三维泡沫制品的方法，所述方法包括下列步骤：
(a)在压力容器中提供包含聚合物的预制件，
(b)使所述预制件在高于大气压的压力下经历至少一种惰性气体，以迫使气体进入所述预制件中，
(c)将所述预制件的温度升高至其软化点以上，其中步骤(b)和(c)可以以任意顺序或同时进行，
(d)将所述压力降低至高于大气压但是低于步骤(b)的所述压力的压力，并且之后将所述预制件冷却至低于其软化点，以得到部分膨胀的制品，
(e)将所述制品转移至第二容器并且在惰性气体或空气的压力下将其加热至高于其软化点的温度，和
(f)在将所述温度维持在等于或高于所述聚合物的软化点的同时降低所述压力，以使所述部分膨胀的制品膨胀而形成发泡制品，
其中所述预制件在至少一个尺寸上的横截面是非均匀的，并且
其中所述预制件由不同材料的区域组成，并且通过不同的交联水平来控制不同区域的膨胀行为以提供相似的膨胀比。
2.根据权利要求1所述的方法，其中所述预制件在至少二个尺寸上的横截面是非均匀的。
3.根据权利要求1所述的方法，其中所述预制件在至少三个尺寸上的横截面是非均匀的。
4.根据权利要求1所述的方法，其中将步骤(d)的所述部分膨胀的制品在转移至步骤(e)的所述第二容器之前储存一段时间。
5.根据权利要求1-4中任一项所述的方法，其中在步骤(a)之前将所述预制件交联。
6.根据权利要求5所述的方法，其中所述交联通过辐射进行。
7.根据前述权利要求1-4和6中任一项所述的方法，其中所述预制件包含一种或多种热塑性树脂。
8.根据前述权利要求5所述的方法，其中所述预制件包含一种或多种热塑性树脂。
9.根据权利要求7所述的方法，其中所述热塑性树脂中的一种或多种是热塑性弹性体(TPE)、聚醚嵌段酰胺(PEBA)或热塑性聚氨酯(TPU)。
10.根据权利要求8所述的方法，其中所述热塑性树脂中的一种或多种是热塑性弹性体(TPE)、聚醚嵌段酰胺(PEBA)或热塑性聚氨酯(TPU)。
11.根据权利要求1-4中任一项所述的方法，其中所述预制件包含用来改变所述聚合物的交联行为的助剂。
12.根据前述权利要求1-4中任一项所述的方法，其中将所述预制件注塑成型。
13.根据权利要求12所述的方法，其中使用重叠注塑、嵌入成型、多喷射注入或共注入方法将所述预制件注塑成型。
14.根据权利要求13所述的方法，其中所述多喷射注入为双喷射注入。
15.根据权利要求1至4中任一项所述的方法，其中使用增材制造方法制造所述预制件。
16.根据权利要求1至4中任一项所述的方法，其中使用3D打印方法制造所述预制件。
17.根据权利要求1-4中任一项所述的方法，其中所述预制件是在一侧上扁平并且具有波状外形轮廓。
18.根据权利要求1-4中任一项所述的方法，其中所述发泡制品的形状具有与所述预制件的形状相同的形式。
19.根据权利要求1-4中任一项所述的方法，其中所述发泡制品的具有相同聚合物组成的区域是均匀的，或者其中所述发泡制品的具有相同聚合物组成的所述区域的化学、热和机械性能是各向同性的。
20.根据权利要求1-4中任一项所述的方法，其中使所述发泡制品经历进一步加工以产生第二3D形状。
21.根据权利要求20所述的方法，其中所述进一步加工是热加工。
22.根据权利要求20所述的方法，其中所述进一步加工是热成形或压缩成型。
23.根据权利要求1-4中任一项所述的方法，其中所述发泡制品是鞋的中底。
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