CN107109038B - 聚对苯二甲酸亚烷基酯树脂组合物 - Google Patents

聚对苯二甲酸亚烷基酯树脂组合物 Download PDF

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Publication number
CN107109038B
CN107109038B CN201580070742.4A CN201580070742A CN107109038B CN 107109038 B CN107109038 B CN 107109038B CN 201580070742 A CN201580070742 A CN 201580070742A CN 107109038 B CN107109038 B CN 107109038B
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polyalkylene terephthalates
formed products
mass
ingredient
resin
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CN107109038A (zh
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坂田耕一
山田真也
山本修央
山本哲朗
松冈佳明
藤本礼久
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Poly Plastics Co., Ltd.
Kaneka Corp
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Kaneka Corp
WinTech Polymer Ltd
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Abstract

本发明涉及一种聚对苯二甲酸亚烷基酯树脂组合物，其包含：(A)聚对苯二甲酸亚烷基酯树脂；以及(B)丙烯酸系核壳型聚合体，其平均粒径为2μm以上，核层成分的含量相对于核层和壳层成分的总量为超过80质量％且不足100质量％。另外，本发明涉及一种由所述聚对苯二甲酸亚烷基酯树脂组合物成形而成的成形品。

Description

聚对苯二甲酸亚烷基酯树脂组合物
技术领域
本发明涉及对苯二甲酸亚烷基酯树脂组合物。具体而言，涉及各种形状的构件的嵌入成形品的耐热冲击性及耐冲击性均均衡性好且优良，而有用于汽车零件、电气、电子零件等的聚对苯二甲酸亚烷基酯树脂组合物。
背景技术
聚对苯二甲酸丁二醇酯树脂(以下也称为“PBT树脂”)等的聚对苯二甲酸亚烷基酯树脂，由于机械性质、电气性质、其他的物理、化学性质优良，且加工性良好，因而作为工程塑料用于汽车零件、电气、电子零件等广泛用途。特别是，可优选用于，以保护从外部的水分、灰尘、或冲击等损坏为目的而收容搭载电子零件的机板的盒材，或内包探测器探针或连接器接头等的嵌入成形品等。
嵌入成形法，是将预先配置在金属模内的金属或无机固体所构成的构件(以下，也称为嵌入构件)，以射出成形的树脂包入的成形法，在可得到充分利用嵌入构件的刚性及导电气，及树脂的赋形性的零件的基础上，由于步骤简单而被广泛地使用。但是，在聚对苯二甲酸亚烷基酯树脂与嵌入构件之间，由温度变化而产生的膨胀收缩率(即线膨胀系数)的差异非常大，因此，树脂部较薄壁的成形品、具有壁厚变化较大的部分的成形品、具有锐角的成形品等，在成形后马上破裂，或因使用中的温度变化而破裂等问题较多。另外，熔融状态的树脂在金属模内绕进嵌入构件汇合时，会形成称为接合的接缝的部分，因此以此作为起点发生龟裂的问题也很多。因此，嵌入成形品的现状是其用途及形状等相当地受限制。
另一方面，对于这些零件，要求进一步改善耐热冲击性，从而可耐用于汽车的引擎室内或屋外等的温度变化严苛的环境下使用，或要求作为框盒使用所需的耐冲击性。对于这些要求，例如，在日本特开2007‐169367号公报公开了在聚对苯二甲酸丁二醇酯树脂中加入设定量的热塑性弹性体或核壳聚合体作为耐冲击改良剂的聚对苯二甲酸丁二醇酯树脂组合物。
另外，日本特开2009‐155448号公报及W02008/032636号公报，分别公开了在聚对苯二甲酸丁二醇酯树脂中加入设定量的核层以丙烯酸系橡胶构成且具有特定粒径的核壳型聚合体，以及玻璃纤维的聚对苯二甲酸丁二醇酯树脂组合物。
(现有技术文献)
(专利文献)
(专利文献1)日本特开2007‐169367号公报
(专利文献2)日本特开2009‐155448号公报
(专利文献3)W02008/032636号公报
发明内容
(发明所要解决的课题)
在日本特开2007‐169367号公报中，使用核壳聚合体，具体是核壳型丙烯酸橡胶作为耐冲击改良剂，使橡胶层的平均粒径为1.0μm以下。本发明人研究表明，此时，包含壳层的核壳整体的平均粒径为1μm左右的小，包含这样的粒径小的核壳型丙烯酸橡胶的聚对苯二甲酸亚烷基酯树脂组合物虽然耐冲击性优良，但耐热冲击性低。另外还发现，假设极端增大壳层的比例，尽管核壳整体的平均粒径变大，含有这样的核层成分比例小的核壳型丙烯酸橡胶的聚对苯二甲酸亚烷基酯树脂组合物，耐热冲击性低。
另外，在日本特开2009‐155448号公报与W02008/032636号公报中，虽然使用平均粒径为2μm以上的核壳型聚合体，但本发明人研究发现，这样的核壳型聚合体，在未适当选择核层与壳层的结构时，存在无法得到充分的耐热冲击性的改善效果的问题。特别是，在嵌入构件的形状使用板状物时，即使是被认为对日本特开2009‐155448号公报的实施例中使用的块状嵌入构件有利的组合物，也确认耐冲击性并不充分。
本发明的实施方式是为解决以上的课题而作出的，其目的在于提供一种用于得到聚对苯二甲酸亚烷基酯树脂组合物的技术，其在由各种形状的嵌入构件的而得到的嵌入成形品中，耐热冲击性及耐冲击性均均衡性好且优良。
(用于解决课题的手段)
本发明人为解决所述课题而深入研究。结果发现使用含有平均粒径为2μm以上且核层成分的含量相对于核层和壳层成分的总量为超过80质量％且不足100质量％的丙烯酸系核壳型聚合体的聚对苯二甲酸亚烷基酯树脂组合物时，耐热冲击性及耐冲击性均均衡性好且优良，从而完成本发明。更具体而言，本发明的实施方式，是涉及下述的聚对苯二甲酸亚烷基酯树脂组合物及成形品。
(1)一种聚对苯二甲酸亚烷基酯树脂组合物，其包含：(A)聚对苯二甲酸亚烷基酯树脂；以及(B)丙烯酸系核壳型聚合体，其平均粒径为2μm以上，核层成分的含量相对于核层和壳层成分的总量为超过80质量％且不足100质量％。
(2)如(1)所述的聚对苯二甲酸亚烷基酯树脂组合物，其中所述(B)成分的平均粒径为2.5μm以上20μm以下，核层成分的含量相对于核层和壳层成分的总量为85质量％以上95质量％以下。
(3)如(1)所述的聚对苯二甲酸亚烷基酯树脂组合物，其中所述(B)成分的平均粒径为3μm以上10μm以下，核层成分的含量相对于核层和壳层成分的总量为90质量％以上92质量％以下。
(4)如(1)所述的聚对苯二甲酸亚烷基酯树脂组合物，其中所述(B)成分的平均粒径为约3μm，核层成分的含量相对于核层和壳层成分的总量为约90质量％。
(5)如(1)至(4)中的任何一项所述的聚对苯二甲酸亚烷基酯树脂组合物，其中相对于100质量份的所述(A)成分，所述(B)成分的含量为10质量份以上50质量份以下。
(6)如(1)至(5)中的任何一项所述的聚对苯二甲酸亚烷基酯树脂组合物，其中相对于100质量份的所述(A)成分，还含有(C)填充剂为10质量份以上100质量份以下。
(7)如(1)至(6)中的任何一项所述的聚对苯二甲酸亚烷基酯树脂组合物，其中在制作下述嵌入成形品A时，满足下述耐热冲击性条件A：
嵌入成形品A：
嵌入成型品的树脂部为宽25mm×70mm×70mm、厚3.6mm的L型板状，嵌入有宽21mm×90mm×90mm、厚1.6mm的L型铁板，一部分的树脂部的最小壁厚为1mm，
耐热冲击性条件A：
使用冷热冲击试验机，以在140℃加热1小时30分钟后，降温至‐40℃冷却1小时30分钟，再升温至140℃的过程作为1个循环的耐热冲击试验，在该耐热冲击试验中，成形品发生龟裂前的循环次数为100以上。
(8)如(1)至(6)中的任何一项所述的聚对苯二甲酸亚烷基酯树脂组合物，其中在制作下述嵌入成形品B时，满足下述耐热冲击性条件B：
嵌入成形品B：
嵌入成形品的树脂部为宽25mm×l20mm、厚4mm的I型板状，嵌入有宽20mm×150mm、厚1.6mm的I型铁板，一部分的树脂部的最小壁厚为1mm，
耐热冲击性条件B：
使用冷热冲击试验机，以在140℃加热1小时30分钟后，降温至‐40℃冷却1小时30分钟，再升温至140℃的过程作为1个循环的耐热冲击试验，在该耐热冲击试验中，成形品发生龟裂前的循环次数为40以上。
(9)一种成形品，其由如(1)至(8)中的任何一项所述的聚对苯二甲酸亚烷基酯树脂组合物成形而成。
(10)如(9)所述的成形品，其为将所述聚对苯二甲酸亚烷基酯树脂组合物，及金属或无机固体形成的嵌入构件嵌入成形而成的嵌入成形品。
(11)如(10)所述的成形品，其中所述嵌入构件为板状的电连接导体。
(12)如(11)所述的成形品，其中所述板状的电连接导体的嵌入构件，在与板状平面的长边方向垂直的剖面上，宽度的最大值与厚度的最大值之比为2以上。
(发明效果)
根据本发明的实施方式，能够得到与各种形状的嵌入构件的嵌入成形品，耐热冲击性及耐冲击性均均衡性好且优良的聚对苯二甲酸亚烷基酯树脂组合物。
附图说明
图1是表示使用在实施例的耐热冲击性评价中制造的棱柱状的嵌入构件的嵌入成形品的立体图(部分透视图)。
图2是表示图1所示嵌入成形品的图，(b)为上侧面图，(a)为沿(b)中的IIa‐IIa线的剖面图。
图3是表示在实施例的耐热冲击性评估所制造的板状(L型)嵌入构件的上面图。
图4是表示使用图3所示板状(L型)嵌入构件的嵌入成形品的图，(a)为上侧面图，(b)为沿(a)的IVb‐IVb线的剖面图，(c)为沿(a)的IVc‐IVc线的剖面图。
图5是表示在实施例的耐热性评估所制造的板状(I型)嵌入构件的上侧面图。
图6是表示使用图5所示的板状(I型)嵌入构件的嵌入成形品的图，(b)是沿(a)的VIb‐VIb线的剖面图，(c)为沿(a)的VIc‐VIc线的剖面图。
具体实施方式
以下详细说明关于本发明的实施方式。但本发明不限于以下的实施方式。
＜聚对苯二甲酸亚烷基酯树脂组合物＞
本发明的实施方式的聚对苯二甲酸亚烷基酯树脂组合物，含有：(A)聚对苯二甲酸亚烷基酯树脂；及(B)丙烯酸系核壳型聚合体，其平均粒径为2μm以上，核层成分的含量相对于核层和壳层成分的总量为超过80质量％不足100质量％。以下说明包含于聚对苯二甲酸亚烷基酯树脂组合物中的各成分。
(A)聚对苯二甲酸亚烷基酯树脂
关于本发明的实施方式的聚对苯二甲酸亚烷基酯树脂组合物的基础树脂的(A)聚对苯二甲酸亚烷基酯树脂，是在以二羧酸化合物及/或其酯形成性衍生物为主成分的二羧酸成分，与以二醇化合物及/或其酯形成性衍生物为主成分的二醇成分反应而得到的热塑性聚酯树脂中，以对苯二甲酸及/或其酯形成性衍生物为主成分而作为二羧酸成分，以亚烷基二醇及/或其酯形成性衍生物为主成分而作为二醇成分的物质。
作为聚对苯二甲酸亚烷基酯树脂，也可使用除主成分以外的二羧酸成分或二醇成分，进一步地，作为其他可共聚的单体的羧酸成分、内酯成分等(以下，有称为共聚合性单体的情况)组合而成的共聚酯。
主成分以外的二羧酸成分，可举例如，脂肪族二羧酸(例如琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、王二酸、癸二酸、十一烷二羧酸、十二烷二羧酸、十六烷二羧酸、二聚酸等的C4‐40左右的二羧酸、优选C4‐14左右的二羧酸)；脂环族二羧酸(例如六氢邻苯二甲酸、六氢间苯二甲酸、六氢对苯二甲酸、5‐双环庚烯‐2，3‐二羧酸等的C4‐40左右的二羧酸，优选C8‐12左右的二羧酸)；对苯二甲酸以外的芳香族二羧酸(例如邻苯二甲酸、间苯二甲酸、甲基间苯二甲酸、甲基对苯二甲酸、2，6‐萘二羧酸等的萘二羧酸、4，4’‐联苯二羧酸，4，4’‐二苯氧基醚二羧酸、4，4’‐二氧安息香酸、4，4’‐二苯基甲烷二羧酸、4，4’‐二苯酮二羧酸等的C8‐16左右的二羧酸)，或这些衍生物(例如，低级烷基酯、芳基酯、酸酐等的可形成酯的衍生物)。适合与对苯二甲酸组合使用的二羧酸成分，可举例间苯二甲酸、萘二羧酸等，也可将上述物质的二种以上组合使用。但是，作为共聚合性单体的二羧酸成分总体优选50摩尔％以上，更优选80摩尔％以上，特别优选90摩尔％以上为芳香族二羧酸化合物。另外，也可按照需要合用偏苯三酸、均苯四甲酸等多元羧酸或其酯形成衍生物(醇酯等)等。合用这样的多官能性化合物，也可得到分枝状的聚对苯二甲酸亚烷基酯树脂。
主成分以外的二醇成分，可举出脂肪族烷二醇(例如，乙二醇、三亚甲基二醇、丙二醇、1，4‐丁二醇、1，3‐丁二醇、新戊二醇、己二醇、辛二醇、癸二醇等的C2‐12左右的脂肪族二醇、优选在C2‐10左右的脂肪族二醇之中，除作为主成分使用以外的脂肪族烷二醇)；聚氧亚烷基二醇(具有多个C2‐4左右的氧亚烷基单元的二醇，例如二甘醇、二丙二醇、二‐四亚甲基二醇、三乙二醇、三丙二醇、聚四亚甲基二醇等)；脂环族二醇(例如，1，4‐环己烷二醇、1，4‐环己烷二甲醇、氢化双酚A等)等。另外，也可合用对苯二酚、间苯二酚、双酚、2，2‐双(4‐羟基苯基)丙烷、2，2‐双‐(4‐(2‐羟基乙氧基)苯基)丙烷、二甲苯二醇等芳香族二醇。但是，作为共聚单体的二醇成分总体，优选50摩尔％以上，更优选80摩尔％以上，特别优选90摩尔％以上为亚烷基二醇。另外，也可根据需要，合用甘油、三羟甲基丙烷、三羟甲基乙烷、异戊四醇等的多元醇或其酯形成性衍生物。合用这样的多官能性化合物，也可得到分枝状的热塑性聚酯树脂。
氧羧酸(或氧羧酸成分或氧羧酸类)，可举例如，氧安息香酸、氧萘酸、羟基苯基酯酸、二醇酸、氧己酸等的氧羧酸或这些衍生物等。内酯，可举丙内酯、丁内酯、戊内酯、己内酯(例如，ε‐己内酯等)等的C3‐12内酯等。
另外，在共聚酯中，共聚合性单体的比例，例如可选自0.01摩尔％以上30摩尔％以下左右的范围，通常为1摩尔％以上25摩尔％以下左右，优选3摩尔％以上20摩尔％以下左右，更优选5摩尔％以上15摩尔％以下左右。另外，均聚酯与共聚酯组合使用时，均聚酯与共聚酯的比例，共聚合性单体与全部单体的比例为0.01摩尔％以上30摩尔％以下(优选1摩尔％以上25摩尔％以下左右，更优选3摩尔％以上20摩尔％以下左右更佳，特别优选5摩尔％以上15摩尔％以下左右)的范围，通常可选自前者/后者＝99/1～1/99(质量比)，优选95/5～5/95(质量比)，优选90/10～10/90(质量比)左右的范围。
在优选的聚对苯二甲酸亚烷基酯树脂中，包含以对苯二甲酸亚烷基酯单元为主成分(例如50～100摩尔％，优选75～100摩尔％左右)的均聚酯或共聚酯(例如，聚对苯二甲酸乙二醇酯(PET)、聚对苯二甲酸三亚甲基酯(PTT)、聚对苯二甲酸丁二醇酯(PBT)等的聚C2‐4对苯二甲酸亚烷基酯)的均聚酯；在以苯二甲酸亚烷基酯单元为主成分的共聚合成分中含有间苯二甲酸亚烷基酯单元的共聚酯、以对苯二甲酸亚烷基酯单元为主成分的共聚合成分中含有萘二甲酸亚烷基酯单元的共聚酯)，这些物质可以单独1种或组合2种以上使用。
特别优选的聚对苯二甲酸亚烷基酯树脂是包含80摩尔％以上(特别是以90摩尔％以上)的对苯二甲酸乙二醇酯、对苯二甲酸三亚甲基酯、对苯二甲酸四亚甲基酯等的C2‐4对苯二甲酸亚烷基酯单元的均聚酯树脂或共聚酯树脂(例如聚对苯二甲酸乙二醇酯树脂、聚对苯二甲酸三亚甲基酯树脂、聚对苯二甲酸丁二醇酯树脂、间苯二甲酸变性聚对苯二甲酸乙二醇酯树脂、间苯二甲酸变性聚对苯二甲酸三亚甲基酯树脂、间苯二甲酸变性聚对苯二甲酸丁二醇酯树脂、萘二羧酸变性聚对苯二甲酸乙二醇酯树脂、萘二羧酸变性聚对苯二甲酸三亚甲基酯树脂、萘二羧酸变性聚对苯二甲酸丁二醇酯树脂等)。
在这些物质中，优选聚对苯二甲酸乙二醇酯树脂、聚对苯二甲酸丁二醇酯树脂，特别优选聚对苯二甲酸丁二醇酯树脂。
聚对苯二甲酸亚烷基酯树脂的末端羧基量，只要不阻碍本发明的效果，并无特别限定。聚对苯二甲酸亚烷基酯树脂的末端羧基量，优选30meq/kg以下，更优选25meq/kg以下。聚对苯二甲酸亚烷基酯树脂的末端羧基量过多，可能损伤耐水解性。
聚对苯二甲酸亚烷基酯树脂的固有粘度(IV)在不阻碍本发明的效果的范围内并无特别限定。聚对苯二甲酸亚烷基酯树脂的固有粘度，优选0.6～l.3dL/g，更优选0.7～1.2dL/g。使用该范围的固有粘度的聚对苯二甲酸亚烷基酯树脂时，所得聚对苯二甲酸亚烷基酯树脂组合物会成为成形性特别优良的物质。另外，也可混合具有不同的固有粘度的聚对苯二甲酸亚烷基酯树脂，调整固有粘度。例如，由混合固有粘度为1.0dL/g的聚对苯二甲酸亚烷基酯树脂与固有粘度为0.8dL/g的聚对苯二甲酸亚烷基酯树脂，能制造固有粘度为0.9dL/g的聚对苯二甲酸亚烷基酯树脂。聚对苯二甲酸亚烷基酯树脂的固有粘度(IV)，例如可在邻氯酚中，以温度35℃的条件测定。
另外，聚对苯二甲酸亚烷基酯树脂也可使用市售品，也可使用将二羧酸成分或其反应性衍生物、二醇成分或其反应性衍生物、以及根据需要可共聚合的单体，以惯用的方法，例如酯交换、直接酯化法等共聚合(聚缩合)而制造的物质。
(B)丙烯酸系核壳型聚合体
核壳型聚合体是具有包含核层(核部)及包覆该核层(核层的表面)的一部分或全部的壳层的多层架构的聚合体。在核壳型聚合体中，优选核层及壳层之中的任意一方，以橡胶成分(软质成分)构成，另一方的成分由硬质成分构成。
核层，通常以橡胶成分构成的情况较多，在本发明的实施方式中，优选使用丙烯酸系橡胶。橡胶成分的玻璃转移温度，例如优选0℃以下(例如，‐10℃以下)，更优选以‐20℃以下(例如‐180～‐25℃左右)进一步优选‐30℃以下(如‐150～‐40℃左右)。
可用于作为橡胶成分的丙烯酸系橡胶，是以丙烯酸系单体(特别是，丙烯酸烷基酯(丙烯酸丁酯等丙烯酸C1～C12烷基酯，优选丙烯酸C1～C8烷基酯，更优选丙烯酸C2～C6烷基酯)等丙烯酸酯)为主成分的聚合体。丙烯酸系橡胶可为丙烯酸烯单体单独或共聚物(丙烯酸系单体的相互的共聚物、丙烯酸系单体与其他的含有不饱和键的单体的共聚物等)，也可为丙烯酸系单体(及其他的含有不饱和键的单体)的架桥性单体的共聚物。
架桥性单体，可举例如(甲基)丙烯酸系单体(多官能性(甲基)丙烯酸酯(例如，二(甲基)丙烯酸丁二醇酯等的(甲基)丙烯酸亚烷基酯；二(甲基)丙烯酸乙二醇酯、二(甲基)丙烯酸丁二醇酯、聚(或寡聚)(甲基)丙烯酸乙二醇酯(二(甲基)丙烯酸二甘醇酯、二(甲基)丙烯酸三乙二醇等)、三(甲基)丙烯酸甘油酯、三羟甲基乙烷三(甲基)丙烯酸酯、三羟甲基丙烷二(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、二(甲基)丙烯酸异戊四醇酯、四(甲基)丙烯酸异戊四醇酯、四(甲基)丙烯酸二异戊四醇酯、六(甲基)丙烯酸二异戊四醇酯等的(多)羟基烷聚(甲基)丙烯酸酯等)的乙烯基烯单体(例如，(甲基)丙烯酸乙烯酯、二乙烯基苯等)；(甲基)丙烯酸缩水甘油酯等)、具有聚合性不饱和键结的水解缩合性化合物(例如，具有(甲基)丙烯酰基的硅烷偶合剂(3‐三甲氧基丙基(甲基)丙烯酸酯等的(甲基)丙烯酰氧烷基三烷氧基硅烷等)等)、丙烯酸系化合物(例如，(甲基)丙烯酸烯丙酯、马来酸二烯丙酯、富马酸二烯丙酯、依康酸二烯丙酯、马来酸单烯丙酯、富马酸单烯丙酯、(异)氰脲酸三烯丙酯等)等。这些架桥性单体，可以单独或组合2种以上使用。
在丙烯酸系橡胶中，丙烯酸酯(特别是，烷基丙烯酸酯)与丙烯酸系橡胶全体的比例，例如优选50～100质量％，更优选70～99质量％，进一步优选80～98质量％左右。另外，在丙烯酸系橡胶中，相对于丙烯酸酯100质量份，架桥性单体例如优选0.1～10质量份，更优选0.2～5质量份，进一步优选0.3～5质量份左右。
另外，核层，即使在以丙烯酸系橡胶为主成分的情况下，也可进一步包含非橡胶成分(例如，后述的硬质树脂成分)。核层的结构，可为均一的结构，也可为不均一的结构(意式腊肠结构等)。
在核壳型聚合体中，壳层通常以硬质树脂成分(或玻璃状树脂成分)构成的情况较多。硬质树脂成分的玻璃转移温度，例如可选自0℃以上(例如，20℃以上)的范围，例如30℃以上(例如30～300℃左右)，优选50℃以上(例如60～250℃左右)，进一步优选70℃以上(例如80～200℃左右)。
这样的硬质树脂成分，通常以乙烯基烯聚合物(乙烯基系单体的聚合物)构成。在乙烯基系聚合物(树脂)中，乙烯基系单体(乙熔基君主单体)，只要是能将乙烯基系聚合物调整为如上所述的玻璃转移温度，并无特别限定，例如在甲基丙烯酸系单体(例如，甲基丙烯酸烷基酯(例如，甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯、甲基丙烯酸己酯，甲基丙烯酸‐2‐乙基己基酯等甲基丙烯酸C1～C20烷基酯，优选甲基丙烯酸C1～C10烷基酯，优选甲基丙烯酸C1～C6烷基酯)、甲基丙烯酸芳酯(甲基丙烯酸苯酯等)、甲基丙烯酸环酯(甲基丙烯酸环己酯等)等的甲基丙烯酸酯等)等之外，可举出上述单体(例如，丙烯酸系单体、芳香族乙烯基系单体(例如，苯乙烯等)、烯烃系单体、氰化乙烯基系单体(例如(甲基)丙烯腈等))等。这些乙烯基系单体，可以单独或组合2种以上使用。乙烯基系单体，多数以选自甲基丙烯酸系单体、芳香族乙烯基系单体、氰化乙烯基系单体中的至少1种(特别是，至少为甲基丙烯酸酯(甲基丙烯酸甲酯等甲基丙烯酸烷酯等))为聚合成分的聚合物。
壳层，只要包覆核层的一部分或全部，可由单层，也可由多层形成。
在核壳型聚合体中，核层成分与核层与壳层的总计的比例，优选为超过80质量％不足100质量％，更优选85质量％以上95质量％以下(例如约90质量％)，进一步优选90质量％以上92质量％以下。核层的比例超过80质量％，则容易得到充分的耐热冲击性的改善效果。核层的比例在95质量％以下，则在制造核壳型聚合体的难易度方面有利，因此在取得性及质量稳定性方面较好。另外，核层与壳层的各成分的比例，可由1HNMR图谱中的来自于各构成成分的波峰部的积分值而计算并分析确认，但通常会大致与制造核壳型聚合体时的各单体调配比例一致，因此可以此作为基础而计算。
在本发明的实施方式中，(B)核壳型聚合体，是在壳层成分具有反应性官能团时，还由于树脂组合物的耐冲击性及耐热冲击性优良，耐水解性特别优良而优选。
所述反应性官能团的种类，可举出环氧基、羟基、羧基、烷氧基、异氰酸酯基、酸酐基、酸氯化物基等，其中优选环氧基。所述反应性官能团的量与100g核壳型聚合体的比例，优选1mmol以上40mmol以下，更优选以2mmol以上20mmol以下，进一步优选3mmol以上15mmol以下。具有1mmol以上的官能团，使耐冲击性有更优良的趋势。另一方面，在40mmol以下时，由于树脂组合物的流动性有不易下降的趋势而优选。
在本发明的实施方式中，相对于100质量份(A)聚对苯二甲酸亚烷基酯树脂，(B)核壳型聚合体的含量优选5质量份以上50质量份以下，更优选10质量份以上30质量份以下。通过使其在该范围内，能够不过多损伤所得聚对苯二甲酸亚烷基酯树脂组合物的耐水解性或流动性，而可改善耐热冲击性。
在本发明的实施方式中，(B)核壳型聚合体的平均粒径优选2μm以上，更优选2.5μm以上20μm以下(例如约3μm左右)，进一步优选3μm以上10μm以下。平均粒径在2μm以上时，容易得到充分的耐热冲击性改善效果，可平衡良好地提升耐热冲击性及耐冲击性。平均粒径在20μm以下时，相对较容易制造核壳型聚合体，在制造成本方面为优选。另外，平均粒径在20μm以下，则所得聚对苯二甲酸亚烷基酯树脂组合物耐水解性优良而特别优选。另外，本发明所述的“平均粒径”是指将乳胶状态的核壳型聚合体使用日机装株式会社制MICROTRACUPA150测定的体积平均粒径(μm)。
这样的核壳型聚合体，特别是壳层以硬质成分构成时，因为由硬质成分的壳而使粒径稳定，因此可抑制在挤出时或成形时的熔融混练条件而引起的聚对苯二甲酸亚烷基酯树脂组合物中的分散状态(平均粒径)的偏差，对其他的弹性体较有利。
((C)填充剂)
本发明的实施方式的聚对苯二甲酸亚烷基酯树脂组合物，也可含有(C)填充剂。含有(C)填充剂可提升机械性能。由降低聚对苯二甲酸亚烷基酯树脂组合物的成形收缩率或线膨胀系数，可期待进一步提升耐热冲击性。
(C)成分的填充剂，包含纤维状填充剂(例如，玻璃纤维、石棉纤维、碳纤维、二氧化硅纤维、氧化铝纤维、硅酸铝纤维、氧化锆纤维、氮化硼纤维、氮化硅纤维、硼纤维、钛酸钾纤维、碳化硅纤维、晶须(碳化硅、氧化铝、氮化硅等的晶须)等的无机质纤维，或以聚酰胺或氟树脂等形成的有机纤维等)；板状填充剂(例如，滑石、云母、玻璃片、石墨等)；粉状填充剂(例如，玻璃珠、玻璃粉、研磨纤维(玻璃等的研磨纤维)、硅酸钙岩矿等)，在这些填充剂中，优选玻璃系填充剂(玻璃纤维、玻璃片、玻璃珠等)、滑石、云母、硅酸钙岩矿等，其中玻璃纤维，在取得性、强度及刚性方面，可良好地适用。另外，板状或粉状的填充剂，在抑制聚对苯二甲酸亚烷基酯树脂组合物的成形收缩率及线膨胀系数的异向性方面，可良好地适用。在使用这些填充剂时，可根据需要使用公知的表面处理剂。
使用纤维状填充剂作为(C)成分时，其形状虽无特别限定，例如长度，优选100μm～5mm，更优选500μm～3mm左右，直径例如，优选l～50μm，更优选3～30μm左右。另外，使用板状填充剂或粉状填充剂时，其平均粒径并无特别限定，例如优选0.1～l00μm，更优选0.1～50μm左右更佳。这些(C)填充剂，可以1种单独或组合2种以上使用。
相对于(A)聚对苯二甲酸亚烷基酯树脂100质量份，(C)成分填充剂的添加量优选10质量份以上100质量份以下，更优选20质量份以上90质量份以下，进一步优选30质量份以上80质量份以下(例如40～70质量份)左右。通过使其在该范围内，不会对树脂组合物的流动性有大的影响，并可提高机械性能。
(其他的成分)
在不妨碍本发明的效果的范围内，为了对本发明的实施方式中的聚对苯二甲酸亚烷基酯树脂组合物赋予所期望的特性，可以配合一般添加于热塑性树脂及热硬化性树脂的公知的物质，例如，抗氧化剂、紫外线吸收剂等稳定剂、耐水解改善剂(例如，环氧树脂等)、防静电剂、阻燃、阻燃助剂、抗滴落剂、染料或颜料等着色剂、脱模剂、润滑剂、结晶促进剂、结晶核剂等。
(配制方法)
本发明的实施方式的聚对苯二甲酸亚烷基酯树脂组合物，可使用以往一般用于配制树脂组合物的设备及方法简单地配制。例如，将各成分混合之后，由单轴或双轴的挤出机混炼，挤出配制胶粒，此后，进行成形的方法；先配制组成不同的胶粒，将该胶粒以既定量混合以供成形，成形后得到目标组成的成形品的方法；以及将各成分的1种或2种以上直接投入成形机的方法等，均可使用。
＜成形品＞
本发明的实施方式的成形品，是将本发明的聚对苯二甲酸亚烷基酯树脂组合物成形而成。成形方法并无特别限定，可采用公知的成形方法。关于本发现的实施方式的成形品，优选将本发明的聚对苯二甲酸亚烷基酯树脂组合物与由金属或无机固体形成的嵌入构件嵌入成形而成的嵌入成形品。金属及无机固体并无特别限定，金属，可示例为铝、镁、不锈钢、钢等，还包括形成于树脂基板上的电子电路等金属导体部。无机固体，可示例为陶瓷等。嵌入成形，可以公知的方法进行。
如上所述，使用板状的电连接导体作为嵌入构件时，以往存在耐热冲击性不足的情况，但在本发明的实施方式的成形品中，即使在这样的情况下也可得到优良的耐热冲击性。这样的板状的电连接导体，具体可举例为，在垂直于板状的平面的长边方向上的剖面，宽度的最大值与厚度的最大值之比为2以上的导体(例如，汇流条等的配线材料)。
另外，在本发明的实施方式的板状的电连接导体中，优选厚度平均为3mm以下，更优选平均2mm以下。另一方面，板状的电连接导体的厚度的下限值并无特别限定，通常为0.1mm。
另外，在本发明的实施方式的成形品(嵌入成形品的形态)中，包覆板状电连接导体的树脂部的厚度并无特别限定，通常为平均3mm以下，优选平均2mm以下。树脂构件的厚度的下限值并无特别限定，通常为0.1mm。此处，包覆板状的电连接导体的树脂部的厚度是指从嵌入成形品的表面，相对于正下方的电连接导体的表面的垂直方向的长度。另外，电连接导体为其间夹有树脂部的层并在一个嵌入成形品中嵌入多个时，此时的树脂部的厚度，可以为从嵌入成形品的表面至正下方的(最外层的)电连接导体的厚度，或夹于各电连接导体间的树脂部的层的厚度，在这些树脂部的厚度之中，只要任意一个在所述树脂部的厚度的范围内时，期望考虑在该树脂部的耐热冲击性。
树脂部的厚度与电连接导体的厚度之比，当树脂部的比例极端地高(电连接导体过薄)时，有因树脂部的收缩而使电连接导体变形的问题，当树脂部的比例极端地低(树脂部过薄)时，有因树脂的流动性不足而成形不良的问题，根据该观点，优选树脂部：电性连接导体＝1:8～8:1，更优选1:5～5:1。
本发明的实施方式的聚对苯二甲酸亚烷基酯树脂组合物、及使用L型或I型的嵌入构件制造嵌入成形品时，将嵌入构件具体的形状，及对应该形状的耐热冲击性条件的示例表示如下。
(1)L型嵌入构件
在制作下述嵌入成形品A时，满足下述耐热冲击性条件A。
(嵌入成形品A)
嵌入成型品的树脂部为宽25mm×70mm×70mm、厚3.6mm的L型板状，嵌入有宽21mm×90mm×90mm、厚1.6mm的L型铁板，一部分的树脂部的最小壁厚为1mm。
(耐热冲击性条件A)
使用冷热冲击试验机，以在140℃加热1小时30分钟后，降温至‐40℃冷却1小时30分钟，再升温至140℃的过程作为1个循环的耐热冲击试验，在该耐热冲击试验中，成形品发生龟裂前的循环次数为100以上(更优选120以上，特别优选150以上)。
(2)I型嵌入构件
在制作下述嵌入成形品B时，满足下述耐热冲击性条件B。
(嵌入成形品B)
嵌入成形品的树脂部为宽25mm×l20mm、厚4mm的I型板状，嵌入有宽20mm×150mm、厚1.6mm的I型铁板，一部分的树脂部的最小壁厚为1mm。
(耐热冲击性条件B)
使用冷热冲击试验机，以在140℃加热1小时30分钟后，降温至‐40℃冷却1小时30分钟，再升温至140℃的过程作为1个循环的耐热冲击试验，在该耐热冲击试验中，成形品发生龟裂前的循环次数为40以上(更优选50以上，特别优选60以上)。
(实施例)
以下，用实施例更详细地说明本发明，但本发明不限于此。
＜材料＞
﹒(A)聚对苯二甲酸亚烷基酯树脂
WinTechPolymer(株)制PBT树脂，固有粘度0.69dl/g、末端羧基量24meq/kg
﹒(B)丙烯酸系核壳型聚合体
B‐1：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核层的比例为90质量％的丙烯酸烯核壳型聚合体，平均粒径3μm
B‐2：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核层的比例为90质量％的丙烯酸系核壳型聚合体，平均粒径20μm
B‐3：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核壳的比例为90质量％的丙烯酸系核壳型聚合体，平均粒径30μm
B‐4：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核壳的比例为80质量％的丙烯酸系核壳型聚合体，平均粒径0.1μm
B‐5：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核壳的比例为80质量％的丙烯酸系核壳型聚合体，平均粒径0.2μm
B‐6：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核壳的比例为80质量％的丙烯酸系核壳型聚合体，平均粒径0.5μm
B‐7：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核壳的比例为80质量％的丙烯酸系核壳型聚合体，平均粒径1.4μm
B‐8：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核壳的比例为80质量％的丙烯酸系核壳型聚合体，平均粒径3.3μm
B‐9：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯聚合物(乙烯基系共聚物)，核层的比例为80质量％的丙烯酸系核壳型聚合体，平均粒径10.5μm
B‐10：核层使用丙烯酸丁酯聚合物(丙烯酸系橡胶)，壳层使用甲基丙烯酸甲酯/甲基丙烯酸缩水甘油酯共聚物(乙烯基系共聚物)，核层的比里为90质量％，甲基丙烯酸甲酯与甲基丙烯酸缩水甘油酯的比例为9质量％：1质量％的丙烯酸系核壳型聚合体，平均粒径3μm
﹒(C)玻璃纤维
日本电气硝子(株)制，产品名：T‐187
﹒抗氧化剂
BASF日本(株式会社)制，产品名：Irgano×1010
﹒耐水解性改善剂
三菱化学(株)制环氧树脂，产品名：EPIKOTE(エピコート)JER1005K
＜实施例1～4，比较例1～6>
相对于(A)聚对苯二甲酸亚烷基酯树脂100质量份，将各成份以表1所示比例混合后，使用30mmφ的双轴挤出机(日本制钢所制TEX‐30)，在料管温度260℃，吐出量15kg/h，螺杆旋转数的150rpm的条件下熔融混炼挤出，得到由聚对苯二甲酸亚烷基酯树脂组成的胶粒。接着，由该胶粒以射出成形制造各种试验片，进行下述物理性质评估。结果合并表示于表1。
(熔融粘度)
将所述胶粒以140℃干燥3小时之后，按照IS011443的标准，使用Capilograph1B(东洋精密机械制造所公司制)，炉体温度260℃，毛细管φ1mm×20mmL，以剪切速度l000sec‐1测定熔融粘度。
(抗拉强度及抗拉断裂应变)
将所述胶粒以140℃干燥3小时之后，以树脂温度260℃，模具温度80℃，射出时间15秒，冷却时间15秒，射出成形IS03167抗拉试验片，按照IS0527‐1，2的标准，测定抗拉强度及抗拉断裂应变。
(耐冲击性(夏氏冲击强度))
将所述胶粒以成形温度260℃，模具温度80℃射出成形，制作夏氏冲击试验片，遵照IS0179/1eA，以23℃测定夏氏冲击强度。
(耐热冲击性(棱柱状构件))
使用所述胶粒，以树脂温度260℃，模具温度65℃，射出时间25秒，冷却时间10秒，对试验片成形用模具(在长22mm、宽22mm、高28mm的棱柱内部，嵌入长14mm、宽14mm、高24mm的铁芯的模具)，使一部分的树脂部的最小壁厚为1mm，嵌入射出成形，制造嵌入成形品。将制造的嵌入成形品表示于图1、图2。图1所示嵌入成形品10，是铁芯14嵌入在树脂部12的嵌入成形品的立体图，图2是该嵌入成形品的(a)剖面图(沿(b)的IIa‐IIa线的剖面图)，(b)为上表面图。铁芯10，是如图2(a)所示，从底面24～26mm的部分为圆柱。另外，如图2(b)所示，铁芯14的周围的树脂部12的最小壁厚为1mm。另外，填充树脂的针点浇口在图2(a)以箭头表示的树脂部底面的中央位置。对所得嵌入成形品使用冷热冲击试验机以140℃加热1小时30分钟后，降温至‐40℃冷却1小时30分钟，进一步升温至140℃的过程为一个循环的耐热冲击试验，测定直到成形品发生龟裂的循环次数，将5个样品的平均破坏寿命作为耐热冲击性的评估。
(耐热冲击性(L型板状构件))
使用所述胶粒，以树脂温度260℃，模具温度65℃，射出时间25秒，冷却时间10秒，对试验片成形用模具(在宽度25mm×70mm×70mm，厚度3.6mm的L型板状构件内部，嵌入宽21mm×90mm×90mm，厚度1.6mm(剖面的宽/厚比为13.1)的L型铁板的模具)，使一部分的树脂部的最小壁厚为1mm，嵌入射出成形，制造嵌入成形品。将使用的L型板状构件、及制造的嵌入成形品表示于图3、图4。图3表示L型板状构件16的上表面图，图4表示L型板状构件16嵌入在树脂部18的嵌入成形品的上表面图((a))及剖面图((b)、(c))。L型板状构件的两端附近的两个孔是在模具内用于嵌入针而固定的，另外，图4所示树脂部18的孔，是以模具内的针压附固定L型板状构件16，以该状态填充树脂时，树脂绕过针而流动所形成。另外，图4(a)，将填充树脂的侧浇口(宽度：4mm，厚度：3mm)的位置以虚线表示，该侧浇口位于树脂部18的右侧面下端部的上方1mm。对所得的嵌入成形品，使用冷热冲击试验机，以140℃加热1小时30分钟之后，降温至‐40℃冷却l小时30分钟，进一步升温至140℃的过程为一个循环的耐热冲击试验，测定直到成形品发生龟裂的循环次数，将5个样品的平均破坏寿命作为耐热冲击性的评估。
(耐热冲击性(I型板状构件))
使用所述胶粒，以树脂温度260℃，模具温度的℃射出时间25秒，冷却时间10秒，对试验片成形用棋具(在宽度25mm×120mm，厚度4mm的I型板状构件内部，嵌入宽度20mm×l50mm，厚度1.6mm(剖面的宽/厚比为12.5)的I型铁板的模具)，使一部分的树脂部的最小壁厚为1mm，嵌入射出成形，制造嵌入成形品。将使用的I型板状构件、及制造的嵌入成形品表示于图5、图6。图5表示I型板状构件20的上表面图，图6表示I型板状构件20嵌入到树脂部22的嵌入成形品的上表面图((a))及剖面图((b)、(c))。I型板状构件的的两端附近的两个孔是在模具内用于嵌入针而固定的，另外，图6所示树脂部22的孔，是以模具内的针压附固定I型板状构件20，以该状态填充树脂时，树脂绕过针而流动所形成。另外，在图6(a)，将填充树脂的侧浇口(宽度：4mm，厚度：3mm)的位置以虚线表示，该侧浇口位于树脂部22的下侧面左端部的右边11mm。对所得嵌入成形品，使用冷热冲击试验机，以140℃加热1小时30分钟之后，降温至‐40℃冷却1小时30分钟，进一步升温至140℃的过程为一个循环的耐热冲击试验，测定直到成形品发生龟裂的循环次数，将5个样品的平均破坏寿命作为耐热冲击性的评估。
(耐水解性)
将使用于抗拉强度的测定的试验片，以压力釜试验机，以121℃、100％RH的条件处理96小时，在中途每24小时测定处理后的抗拉强度，求出处理前后的保持率。
(表1)
由表1可知，通过使用平均粒径为2μm以上，且核层成分与核层和壳层成分总计的比例超过80质量％的丙烯酸系核壳型聚合体，可不过大损伤耐热冲击性(实施例1～4)。另外，平均粒径小于2μm时，并不一定对耐热冲击性有利(比较例1～3)，另外，即使平均粒径大，但核层的成分在80质量％以下时(比较例4～6)，在棱柱型嵌入构件难以观察到与核层的成分超过80质量％时的差别，在板状嵌入构件，可以观察到显著的差别。另外，平均粒径变得过大则可预期耐热冲击性、耐冲击性及耐水解性会有下降的倾向，因此难以预期得到由本发明限定的范围所得到的效果。
另外，丙烯酸系核壳型聚合体具有反应性官能团时，所得的聚对苯二甲酸亚烷基酯树脂组合物成为耐冲击性与耐热冲击性优良，并且耐水解性特别优良的物质(实施例4)。
日本专利申请2014‐265294的全部公开内容参照包含于本说明书中。
本说明书中记载的所有文献、专利申请、及技术规格，与各个文献、专利申请、及技术规格具体地个别记载情况相同程度地参照包含于本说明书中。
【符号说明】
10 嵌入成形品
12、18、22 树脂部
14 铁芯
16 L型板状构件
20 I型板状构件

Claims (12)

1.一种聚对苯二甲酸亚烷基酯树脂组合物，其包含：
(A)聚对苯二甲酸亚烷基酯树脂；以及
(B)丙烯酸系核壳型聚合体，其平均粒径为2μm以上，核层成分的含量相对于核层和壳层成分的总量为85质量％以上95质量％以下。
2.根据权利要求1所述的聚对苯二甲酸亚烷基酯树脂组合物，其中，所述(B)成分的平均粒径为2.5μm以上20μm以下。
3.根据权利要求1所述的聚对苯二甲酸亚烷基酯树脂组合物，其中，所述(B)成分的平均粒径为3μm以上10μm以下，核层成分的含量相对于核层和壳层成分的总量为90质量％以上92质量％以下。
4.根据权利要求1所述的聚对苯二甲酸亚烷基酯树脂组合物，其中，所述(B)成分的平均粒径为3μm，核层成分的含量相对于核层和壳层成分的总量为90质量％。
5.根据权利要求1或2所述的聚对苯二甲酸亚烷基酯树脂组合物，其中，相对于100质量份的所述(A)成分，所述(B)成分的含量为5质量份以上50质量份以下。
6.根据权利要求1或2所述的聚对苯二甲酸亚烷基酯树脂组合物，其中相对于100质量份的所述(A)成分，还含有(C)填充剂为10质量份以上100质量份以下。
7.根据权利要求1或2所述的聚对苯二甲酸亚烷基酯树脂组合物，其中在制作下述嵌入成形品A时，满足下述耐热冲击性条件A，
嵌入成形品A：
嵌入成型品的树脂部为宽25mm×70mm×70mm、厚3.6mm的L型板状，嵌入有宽21mm×90mm×90mm、厚1.6mm的L型铁板，一部分的树脂部的最小壁厚为1mm，
耐热冲击性条件A：
使用冷热冲击试验机，以在140℃加热1小时30分钟后，降温至-40℃冷却1小时30分钟，再升温至140℃的过程作为1个循环的耐热冲击试验，在该耐热冲击试验中，成形品发生龟裂前的循环次数为100以上。
8.根据权利要求1或2所述的聚对苯二甲酸亚烷基酯树脂组合物，其中在制作下述嵌入成形品B时，满足下述耐热冲击性条件B：
嵌入成形品B：
嵌入成形品的树脂部为宽25mm×l20mm、厚4mm的I型板状，嵌入有宽20mm×150mm、厚1.6mm的I型铁板，一部分的树脂部的最小壁厚为1mm，
耐热冲击性条件B：
使用冷热冲击试验机，以在140℃加热1小时30分钟后，降温至-40℃冷却1小时30分钟，再升温至140℃的过程作为1个循环的耐热冲击试验，在该耐热冲击试验中，成形品发生龟裂前的循环次数为40以上。
9.一种成形品，其由权利要求1至8中的任意一项所述的聚对苯二甲酸亚烷基酯树脂组合物成形而成。
10.根据权利要求9所述的成形品，其为将所述聚对苯二甲酸亚烷基酯树脂组合物，和金属或无机固体形成的嵌入构件嵌入成形而成的嵌入成形品。
11.根据权利要求10所述的成形品，其中所述嵌入构件为板状的电连接导体。
12.根据权利要求11所述的成形品，其中所述作为板状电连接导体的嵌入构件，在与板状平面的长边方向垂直的剖面上，宽度的最大值与厚度的最大值之比为2以上。
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JP2003128736A (ja) * 2001-10-26 2003-05-08 Negami Kogyo Kk アクリル樹脂粒子
CN101910306A (zh) * 2007-12-26 2010-12-08 胜技高分子株式会社 聚对苯二甲酸丁二醇酯树脂组合物

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