CN109328213A - 橡胶组合物、橡胶成型体和橡胶成型体的制造方法 - Google Patents
橡胶组合物、橡胶成型体和橡胶成型体的制造方法 Download PDFInfo
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- CN109328213A CN109328213A CN201780039936.7A CN201780039936A CN109328213A CN 109328213 A CN109328213 A CN 109328213A CN 201780039936 A CN201780039936 A CN 201780039936A CN 109328213 A CN109328213 A CN 109328213A
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- rubber
- alpha
- copolymer rubber
- mass parts
- ethylene
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Abstract
本发明公开一种橡胶组合物,其含有:(A)包含乙烯单元和碳原子数为3以上的α‑烯烃单元的乙烯‑α‑烯烃系共聚物橡胶;(B)包含磷原子和氮原子的阻燃剂;(C)热膨胀性石墨;以及(D)作为多孔粒子或具有离子交换性的粒子的添加粒子。相对于乙烯‑α‑烯烃系共聚物橡胶100质量份,阻燃剂的含量为50~250质量份,添加粒子的含量为15质量份以下。
Description
技术领域
本发明涉及橡胶组合物、橡胶成型体和橡胶成型体的制造方法。
背景技术
以乙烯-α-烯烃共聚物橡胶和乙烯-α-烯烃-非共轭多烯共聚物橡胶为代表的乙烯-α-烯烃系共聚物橡胶被广泛用于汽车部件、电气/电子部件、铁路车辆部件等用途中。
在电气/电子设备用途等中,为了防止因暴露于来自设备内部的发热或者来自外部的高温而使壳体或部件起火、燃烧,材料具有阻燃性很重要。对于铁路车辆等的结构材料而言,为了避免因火灾而着火、燃烧,具有阻燃性也很重要。
以往,为了对橡胶组合物赋予阻燃性,大多使用了卤素系阻燃剂和锑系化合物,但近年来对于不含卤素系阻燃剂的无卤素的橡胶组合物的需求正在扩大。作为不使用卤素系阻燃剂而用于赋予阻燃性的方法,已知在合成树脂中添加以红磷、磷酸系阻燃剂为代表的无机磷系阻燃剂、以多磷酸铵为代表的有机磷系阻燃剂、或者金属氢氧化物系阻燃剂的方法(参照专利文献1~3)。
现有技术文献
专利文献
专利文献1:日本特开2013-18847号公报
专利文献2:日本特开2001-40156号公报
专利文献3:日本特开平6-73237号公报
发明内容
发明要解决的课题
为了提高橡胶成型体的阻燃性,通常需要增加阻燃剂的混配量。但是,混配大量阻燃剂有时会引起由成型工序中的喷霜(bloom)(参照ISO 1382:2012(en)Rubber-Vocabulary(橡胶词汇),2.50bloom)导致的模具污染。因此,伴随着对橡胶组合物所要求的阻燃性水平的进一步提高,具有难以兼顾阻燃性与模具污染的抑制的倾向。
因此,本发明的一个方面的目的在于提供一种橡胶组合物,其尽管具有高阻燃性,但仍然难以产生成型工序中的模具污染。
用于解决课题的方案
本发明的一个方面提供一种橡胶组合物,其含有:
(A)包含乙烯单元和碳原子数为3以上的α-烯烃单元的乙烯-α-烯烃系共聚物橡胶;
(B)包含磷原子和氮原子的阻燃剂;
(C)热膨胀性石墨;以及
(D)作为多孔粒子或具有离子交换性的粒子的添加粒子。
在该橡胶组合物中,相对于(A)乙烯-α-烯烃系共聚物橡胶100质量份,(B)阻燃剂的含量为50~250质量份,(D)添加粒子的含量为15质量份以下。该橡胶组合物尽管具有高阻燃性,但仍然难以产生成型工序中的模具污染。
发明的效果
根据本发明的一个方面,可以提供一种橡胶组合物,其尽管具有高阻燃性,但仍然难以产生成型工序中的模具污染。
附图说明
图1是示出橡胶成型体的一个实施方式的截面图。
具体实施方式
以下,对本发明的实施方式进行说明。但是,本发明不受以下实施方式的限定。
橡胶组合物
一个实施方式的橡胶组合物含有:作为成分(A)的乙烯-α-烯烃系共聚物橡胶;作为成分(B)的包含磷原子和氮原子的阻燃剂;作为成分(C)的热膨胀性石墨;以及作为成分(D)的添加粒子。
成分(A):乙烯-α-烯烃系共聚物橡胶
乙烯-α-烯烃系共聚物橡胶包含乙烯单元和碳原子数为3以上的α-烯烃单元作为主要的单体单元。α-烯烃单元的碳原子数可以为3以上且20以下。相对于共聚物橡胶的总体质量,乙烯-α-烯烃系共聚物橡胶中的乙烯单元与α-烯烃单元的合计含量可以为60质量%以上且100质量%以下、或者80质量%以上且100质量%以下。乙烯-α-烯烃系共聚物橡胶例如可以为实质上由乙烯单元和α-烯烃单元构成的乙烯-α-烯烃共聚物橡胶,也可以为包含乙烯单元、α-烯烃单元和非共轭多烯单元的乙烯-α-烯烃-非共轭多烯共聚物橡胶。本说明书中,像“乙烯单元”、“α-烯烃单元”、“非共轭多烯单元”这样“单体名+单元”的术语是指“基于该单体的单体单元”。
作为构成乙烯-α-烯烃系共聚物橡胶的α-烯烃的具体例,可以举出丙烯、1-丁烯、1-戊烯、1-己烯、1-庚烯、1-辛烯、1-壬烯和1-癸烯等直链状烯烃;3-甲基-1-丁烯、3-甲基-1-戊烯和4-甲基-1-戊烯等支链状烯烃;乙烯基环己烷等环状烯烃。它们可以单独使用或将两种以上组合使用。乙烯-α-烯烃系共聚物橡胶中包含的α-烯烃可以为丙烯或1-丁烯中的至少任一者,也可以为丙烯。
乙烯-α-烯烃系共聚物橡胶中的乙烯单元/α-烯烃单元的质量比没有特别限制,可以为90/10~30/70或85/15~45/55。
相对于共聚物橡胶的总体质量,乙烯-α-烯烃-非共轭多烯共聚物橡胶中的乙烯单元、α-烯烃单元和非共轭多烯单元的合计含量可以为60质量%以上且100质量%以下、或者80质量%以上且100质量%以下。
乙烯-α-烯烃-非共轭多烯共聚物橡胶中的非共轭多烯单元的含量以碘值换算(单位:g/100g共聚物橡胶)计可以为0以上且40以下。通过使非共轭多烯单元的含量以碘值换算计为40以下,所得到的成型体的耐候性能够提高。从同样的观点出发,非共轭多烯单元的含量以碘值换算计可以为0以上且35以下、或者0以上且30以下。
构成乙烯-α-烯烃-非共轭多烯共聚物橡胶的非共轭多烯的碳原子数可以为3以上且20以下。作为非共轭多烯的具体例,可以举出:1,4-己二烯、1,6-辛二烯、2-甲基-1,5-己二烯、6-甲基-1,5-庚二烯、以及7-甲基-1,6-辛二烯等链状非共轭二烯;环己二烯、双环戊二烯、5-乙烯基降冰片烯、5-亚乙基-2-降冰片烯、5-(2-丙烯基)-2-降冰片烯、5-(3-丁烯基)-2-降冰片烯、5-(4-戊烯基)-2-降冰片烯、5-(5-己烯基)-2-降冰片烯、5-(6-庚烯基)-2-降冰片烯、5-(7-辛烯基)-2-降冰片烯、5-亚甲基-2-降冰片烯、以及6-氯甲基-5-异丙烯基-2-降冰片烯等环状非共轭二烯;4-亚乙基-8-甲基-1,7-壬二烯、5,9,13-三甲基-1,4,8,12-十四碳二烯、4-亚乙基-12-甲基-1,11-十五碳二烯、2,3-二亚异丙基-5-降冰片烯、2-亚乙基-3-亚异丙基-5-降冰片烯、2-丙烯基-2,2-降冰片二烯、1,3,7-辛三烯、6,10-二甲基-1,5,9-十一碳三烯、5,9-二甲基-1,4,8-癸三烯、13-乙基-9-甲基-1,9,12-十五碳三烯、5,9,8,14,16-五甲基-1,7,14-十六碳三烯、以及1,4,9-癸三烯等三烯。它们可以单独使用或组合使用。这些之中,乙烯-α-烯烃-非共轭多烯共聚物橡胶可以包含5-亚乙基-2-降冰片烯、双环戊二烯、5-乙烯基降冰片烯或它们的组合。
作为乙烯-α-烯烃系共聚物橡胶的具体例,可以举出乙烯-丙烯共聚物橡胶、乙烯-丙烯-5-亚乙基-2-降冰片烯共聚物橡胶、乙烯-丙烯-双环戊二烯共聚物橡胶、乙烯-丙烯-1,4-己二烯共聚物橡胶、乙烯-丙烯-1,6-辛二烯共聚物橡胶、乙烯-丙烯-2-甲基-1,5-己二烯共聚物橡胶、乙烯-丙烯-6-甲基-1,5-庚二烯共聚物橡胶、乙烯-丙烯-7-甲基-1,6-辛二烯共聚物橡胶、乙烯-丙烯-环己二烯共聚物橡胶、乙烯-丙烯-5-乙烯基降冰片烯共聚物橡胶、乙烯-丙烯-5-(2-丙烯基)-2-降冰片烯共聚物橡胶、乙烯-丙烯-5-(3-丁烯基)-2-降冰片烯共聚物橡胶、乙烯-丙烯-5-(4-戊烯基)-2-降冰片烯共聚物橡胶、乙烯-丙烯-5-(5-己烯基)-2-降冰片烯共聚物橡胶、乙烯-丙烯-5-(6-庚烯基)-2-降冰片烯共聚物橡胶、乙烯-丙烯-5-(7-辛烯基)-2-降冰片烯共聚物橡胶、乙烯-丙烯-5-亚甲基-2-降冰片烯共聚物橡胶、乙烯-丙烯-4-亚乙基-8-甲基-1,7-壬二烯共聚物橡胶、乙烯-丙烯-5,9,13-三甲基-1,4,8,12-十四碳二烯共聚物橡胶、乙烯-丙烯-4-亚乙基-12-甲基-1,11-十五碳二烯共聚物橡胶、乙烯-丙烯-6-氯甲基-5-异丙烯基-2-降冰片烯共聚物橡胶、乙烯-丙烯-2,3-二亚异丙基-5-降冰片烯共聚物橡胶、乙烯-丙烯-2-亚乙基-3-亚异丙基-5-降冰片烯共聚物橡胶、乙烯-丙烯-2-丙烯基-2,2-降冰片二烯共聚物橡胶、乙烯-丙烯-1,3,7-辛三烯共聚物橡胶、乙烯-丙烯-6,10-二甲基-1,5,9-十一碳三烯共聚物橡胶、乙烯-丙烯-5,9-二甲基-1,4,8-癸三烯共聚物橡胶、乙烯-丙烯-13-乙基-9-甲基-1,9,12-十五碳三烯共聚物橡胶、乙烯-丙烯-5,9,8,14,16-五甲基-1,7,14-十六碳三烯共聚物橡胶、以及乙烯-丙烯-1,4,9-癸三烯共聚物橡胶。它们可以单独使用或组合使用。
乙烯-α-烯烃系共聚物橡胶可以包含乙烯-丙烯共聚物橡胶、乙烯-丙烯-5-亚乙基-2-降冰片烯共聚物橡胶、乙烯-丙烯-双环戊二烯共聚物橡胶、乙烯-丙烯-5-乙烯基降冰片烯共聚物橡胶或它们的组合,也可以包含乙烯-丙烯共聚物橡胶和/或乙烯-丙烯-5-亚乙基-2-降冰片烯共聚物橡胶。
橡胶组合物包含2种以上的乙烯-α-烯烃系共聚物橡胶的情况下,上述的乙烯单元/α-烯烃单元的质量比和碘值为在这2种以上的乙烯-α-烯烃系共聚物橡胶的整体中的值。
乙烯-α-烯烃系共聚物橡胶在100℃的门尼粘度(ML1+4、100℃)可以为10~350或30~300。若门尼粘度过小,则橡胶成型体的机械强度有时会降低,若门尼粘度过大,则具有混炼加工性降低的倾向。
乙烯-α-烯烃系共聚物的分子量分布(Mw/Mn)可以为1.5以上且5.0以下。若分子量分布为1.5以上,则容易得到橡胶组合物的良好的辊加工性。若分子量分布为5.0以下,则具有成型体的机械物性提高的倾向。从同样的观点出发,乙烯-α-烯烃系共聚物的分子量分布可以为2.0以上且3.0以下。分子量分布可以通过变更聚合条件来调节。
本说明书中的分子量分布是由利用凝胶渗透色谱法(GPC法)测定的聚苯乙烯换算的重均分子量(Mw)和数均分子量(Mn)算出的比值(Mw/Mn)。作为基于GPC法的重均分子量和数均分子量的测定条件,例如如下所述。
·GPC装置:东曹株式会社制造、商品名HLC-8121GPC/HT
·柱:东曹株式会社制造、商品名TSKgel GMHHR-H(S)HT
·分子量标准物质:分子量为500以上且20,000,000以下的聚苯乙烯
·洗脱溶剂流速:1.0mL/min
·试样浓度:1mg/mL
·测定温度:140℃
·洗脱溶剂:邻二氯苯
·注入量:500μL
·检测器:差示折射计
乙烯-α-烯烃系共聚物也可以与链烷烃系油和环烷烃系油等加工油组合,作为充油橡胶而用于橡胶组合物的制备。
(乙烯-α-烯烃系共聚物橡胶的制造方法)
一个实施方式的乙烯-α-烯烃系共聚物橡胶没有特别限定,例如可以通过包括下述工序的方法进行制造:在所谓齐格勒纳塔催化剂或茂金属催化剂等催化剂的存在下,使包含乙烯、α-烯烃、以及根据需要的非共轭多烯的单体混合物进行共聚。
作为用于共聚的催化剂,优选使用利用下述式(1)所示的钒化合物和下述式(2)所示的有机铝化合物而得到的催化剂。由此,可以容易地制造单体反应性比的乘积更低的乙烯-α-烯烃系共聚物橡胶。
VO(OR)mX3-m·····(1)
[式中,R表示碳原子数为1以上且8以下的直链状烃基,X表示卤素原子,m表示满足0<m≤3的数。]
R”jAlX”3-j·····(2)
[式中,R”表示烃基,X”表示卤素原子,j表示满足0<j≤3的数。]
作为式(1)中的R的具体例,可以举出甲基、乙基、正丙基、正丁基、正戊基和正己基。这些之中,优选碳原子数为1以上且3以下的直链状烷基。作为X,可以举出氟原子、氯原子等。m优选为满足1≤m≤2的数。
作为式(1)所示的钒化合物的具体例,可以举出VO(OCH3)Cl2、VO(OC2H5)Cl2、VO(O(n-C3H7))Cl2、VO(O(n-C4H9))Cl2、VO(O(n-C5H11))Cl2、VO(O(n-C6H13))Cl2、VO(O(n-C7H15))Cl2、VO(O(n-C8H17))Cl2、VO(OCH3)0.5Cl2.5、VO(OC2H5)0.5Cl2.5、VO(O(n-C3H7))0.5Cl2.5、VO(O(n-C4H9))0.5Cl2.5、VO(O(n-C5H11))0.5Cl2.5、VO(O(n-C6H13))0.5Cl2.5、VO(O(n-C7H15))0.5Cl2.5、VO(O(n-C8H17))0.5Cl2.5、VO(OCH3)1.5Cl1.5、VO(OC2H5)1.5Cl1.5、VO(O(n-C3H7))1.5Cl1.5、VO(O(n-C4H9))1.5Cl1.5、VO(O(n-C5H11))1.5Cl1.5、VO(O(n-C6H13))1.5Cl1.5、VO(O(n-C7H15))1.5Cl1.5、VO(O(n-C8H17))1.5Cl1.5、VO(OCH3)0.8Cl2.2、VO(OC2H5)0.8Cl2.2、VO(O(n-C3H7))0.8Cl2.2、VO(O(n-C4H9))0.8Cl2.2、VO(O(n-C5H11))0.8Cl2.2、VO(O(n-C6H13))0.8Cl2.2、VO(O(n-C7H15))0.8Cl2.2、以及VO(O(n-C8H17))0.8Cl2.2、VO(OCH3)1.8Cl1.2、VO(OC2H5)1.8Cl1.2、VO(O(n-C3H7))1.8Cl1.2、VO(O(n-C4H9))1.8Cl1.2、VO(O(n-C5H11))1.8C11.2、VO(O(n-C6H13))1.8Cl1.2、VO(O(n-C7H15))1.8Cl1.2、以及VO(O(n-C8H17))1.8Cl1.2。这些之中,特别优选VO(OC2H5)Cl2、VO(OC2H5)0.5Cl2.5、VO(OC2H5)1.5Cl1.5、VO(OC2H5)0.8Cl2.2、以及VO(OC2H5)1.8Cl1.2。它们可以单独使用或组合使用。
式(1)所示的钒化合物例如可以利用使VOX3与ROH以规定的摩尔比发生反应的方法来获得。例如,VOCl3与C2H5OH的反应由下式表示。也可以将VOX3和ROH供给到聚合槽,在聚合槽中生成式(1)的钒化合物。
VOCl3+m·C2H5OH→VO(OC2H5)mCl3-m+m·HCl
式(2)中的R”可以是碳原子数为1~10的烷基,作为其具体例,可以举出甲基、乙基、正丙基、异丙基、正丁基、异丁基、戊基和己基。作为X”,可以举出氟原子、氯原子等。j优选为满足0<j≤2的数。
作为式(2)所示的有机铝化合物的具体例,可以举出(C2H5)2AlCl、(n-C4H9)2AlCl、(iso-C4H9)2AlCl、(n-C6H13)2AlCl、(C2H5)1.5AlCl1.5、(n-C4H9)1.5AlCl1.5、(iso-C4H9)1.5AlCl1.5、(n-C6H13)1.5AlCl1.5、C2H5AlCl2、(n-C4H9)AlCl2、(iso-C4H9)AlCl2、以及(n-C6H13)AlCl2。这些之中,特别优选(C2H5)2AlCl、(C2H5)1.5AlCl1.5、以及C2H5AlCl2。它们可以单独使用或组合使用。
式(2)的有机铝化合物与式(1)的钒化合物的使用量的摩尔比(有机铝化合物的摩尔/钒化合物的摩尔)优选为0.1以上且50以下、更优选为1以上且30以下、进一步优选为2以上且15以下、特别优选为3以上且10以下。通过调整该摩尔比,可以调整共聚物橡胶的粘度、Mw/Mn和Mz/Mn等。例如,若该摩尔比大,则具有共聚物橡胶的粘度升高的倾向、以及Mw/Mn和Mz/Mn减小的倾向。
聚合反应例如可以通过使用1个聚合槽进行聚合的方法、或者使用串联的2个聚合槽来进行。可以向聚合槽中供给单体、催化剂、以及根据需要的其他成分,在聚合槽中将单体聚合。
聚合反应通常在溶剂中进行。作为聚合中所用的溶剂,例如可以举出丙烷、丁烷、异丁烷、戊烷、己烷、庚烷、辛烷等脂肪族烃;环戊烷、环己烷等脂环族烃等非活性溶剂。它们可以单独使用或组合使用。这些之中,优选脂肪族烃。
聚合温度通常可以为0℃以上且200℃以下,优选为20℃以上且150℃以下、更优选为30℃以上且120℃以下。聚合压力通常可以为0.1MPa以上且10MPa以下,优选为0.1MPa以上且5MPa以下、更优选为0.1MPa以上且3MPa以下。通过调整聚合温度,可以调整成分(A)的Mw/Mn等。例如,若聚合温度低,则具有Mw/Mn减小的倾向。
在聚合时,根据需要,也可以向聚合槽供给作为分子量调节剂的氢。向聚合槽供给的氢量相对于1kg向聚合槽供给的溶剂优选为0.001~0.1NL、更优选为0.005~0.05NL、进一步优选为0.01~0.04NL。通过调整氢的供给量,可以调整乙烯-α-烯烃系共聚物的Mw/Mn、以及粘度等。例如,若氢的供给量多,则具有Mw/Mn减小的倾向。若氢的供给量少,则具有粘度增大的倾向。
相对于向聚合槽供给的溶剂100质量份,向聚合槽供给的钒化合物的量优选为0.002质量份以上且0.2质量份以下、更优选为0.003质量份以上且0.1质量份以下。通过调整相对于溶剂的钒化合物的量,可以调整乙烯-α-烯烃系共聚物橡胶的粘度。例如,通过增加该钒化合物的量,具有能够增大粘度的倾向。
成分(B):包含磷原子和氮原子的阻燃剂
成分(B)的阻燃剂由包含磷原子和氮原子的1种以上化合物构成。该阻燃剂可以包含通常被称为磷系阻燃剂的物质中的具有氨基的化合物。包含磷原子和氮原子的阻燃剂也可以包含由磷酸或多磷酸与亚烷基多胺或聚亚烷基多胺形成的磷酸盐。包含磷原子和氮原子的阻燃剂是与(D)成分的添加粒子不同地包含于橡胶组合物中的成分。
构成磷酸盐的磷酸或多磷酸例如可以为磷酸(正磷酸)、焦磷酸(二磷酸)、三磷酸、四磷酸、偏磷酸(三偏磷酸、四偏磷酸、六偏磷酸等)或它们的组合。
磷酸盐可以包含1种以上的亚烷基多胺和聚亚烷基多胺(下文中有时将它们一并称为“(聚)亚烷基多胺”)。构成磷酸盐的(聚)亚烷基多胺可以为直链状或支链状化合物,也可以为环状化合物。环状的(聚)亚烷基多胺可以为相邻的氮原子彼此键合形成环的化合物。在(聚)亚烷基多胺中,氨基或亚氨基的氢原子可以被取代基(例如甲基、乙基等C1-4烷基等)所取代。
构成磷酸盐的代表性的亚烷基多胺为亚烷基二胺。亚烷基二胺的碳原子数可以为1~20或2~10。作为碳原子数为1~20的亚烷基二胺的例子,可以举出二氨基甲烷、乙二胺、1,2-丙二胺、四亚甲基二胺、五亚甲基二胺、六亚甲基二胺、1,7-二氨基庚烷、1,8-二氨基辛烷、1,9-二氨基壬烷、1,10-二氨基癸烷、以及吡唑烷。
作为构成磷酸盐的聚亚烷基多胺,例如可以举出二亚烷基多胺、三亚烷基多胺、四亚烷基多胺、五亚烷基多胺、六亚烷基多胺、七亚烷基多胺和八亚烷基多胺。各亚烷基的碳原子数可以为2~10、2~6或2~4。作为聚亚烷基多胺的具体例,可以举出二亚乙基三胺、哌嗪、2,5-二甲基哌嗪、1,4-双(氨基乙基)哌嗪、三亚乙基四胺、以及四亚乙基五胺。
作为包含磷原子和氮原子的阻燃剂的市售品,有株式会社ADEKA制造的“ADK STABFP-2100JC”、株式会社ADEKA制造的“ADK STAB FP2200”、株式会社ADEKA制造的“ADK STABFP2200S”。
相对于乙烯-α-烯烃系共聚物100质量份,橡胶组合物中的包含磷原子和氮原子的阻燃剂的含量典型地为50~250质量份,可以为80~200质量份或80~150质量份。若包含磷原子和氮原子的阻燃剂的含量多,则具有阻燃性提高的倾向。若包含磷原子和氮原子的阻燃剂的含量过多,则具有加工性降低的倾向。
成分(C):热膨胀性石墨
热膨胀性石墨与成分(B)的阻燃剂的组合能够有助于橡胶成型体的高阻燃性。如本领域技术人员所理解的那样,热膨胀性石墨是包含具有层状结构的石墨和配置在该层状结构的层间的层间化合物的材料。热膨胀性石墨例如通过将天然鳞状石墨、热解石墨、漂浮石墨等的粉末用浓硫酸、硝酸、硒酸等无机酸与浓硝酸、高氯酸、高氯酸盐、高锰酸盐、重铬酸盐、过氧化氢等强氧化剂进行处理的方法来获得。特别是,成分(B)可以为在进行酸处理后进而用氨、脂肪族低级胺、碱金属化合物、碱土金属化合物中和而得到的热膨胀性石墨。作为热膨胀性石墨的市售品,有AIR WATER INC.制造的“MZ-260”、AIR WATER INC.制造的“CA-60N”。热膨胀性石墨是与(D)成分的添加粒子不同地包含于橡胶组合物中的成分。
相对于乙烯-α-烯烃系共聚物100质量份,橡胶组合物中的热膨胀性石墨的含量典型地为1~100质量份,可以为5~70质量份。若热膨胀性石墨的含量多,则具有阻燃性提高的倾向。若热膨胀性石墨的含量过多,则具有加工性降低的倾向。
成分(D):添加粒子
作为成分(D)使用的添加粒子能够为多孔粒子或具有离子交换性的粒子。添加粒子也可以为具有离子交换性的多孔粒子。即,作为成分(D)使用的添加粒子能够为多孔粒子、具有离子交换性的粒子、或者具有离子交换性的多孔粒子。可认为这些添加粒子通过在成型工序中吸附橡胶组合物中产生的喷霜物而有助于抑制模具污染。多孔粒子能够基于其多孔的形态而作为吸附材料发挥功能。具有离子交换性的粒子通过基于离子交换性而与喷霜物发生相互作用,能够作为吸附材料发挥功能。
作为添加粒子的多孔粒子可以为无机粒子。多孔粒子例如可以为选自由二氧化硅粒子、氧化镁粒子、氧化钛粒子、硅酸钙粒子、硅酸镁粒子和活性炭组成的组中的至少1种。作为添加粒子的具有离子交换性的粒子也可以为无机粒子。具有离子交换性的粒子例如可以为选自由水滑石粒子、沸石粒子、锆粒子、氧化铝粒子、高岭石粒子、埃洛石粒子、蒙脱石粒子、蛭石粒子、蒙脱土粒子、伊毛缟石粒子、水铝英石粒子、三水铝石粒子和丝光沸石粒子组成的组中的至少1种。作为添加粒子,可以使用选自它们中的至少1种粒子。添加粒子可以为二氧化硅粒子、水滑石粒子或它们的组合。由此,关于模具污染的抑制能够得到特别优异的效果。
相对于乙烯-α-烯烃系共聚物100质量份,成分(D)的添加粒子的含量典型地为15质量份以下。通过使该含量为15质量份以下,尽管可维持特别高的阻燃性,但仍然能够抑制成型工序中的模具污染。从同样的观点出发,该含量可以为10质量份以下或5质量份以下。相对于乙烯-α-烯烃系共聚物100质量份,添加粒子的含量可以为0.5质量份以上或1质量份以上。若添加剂的含量多,则具有抑制模具污染的效果增大的倾向。
(其他成分)
除了以上说明的成分以外,本实施方式的橡胶组合物可以在不显著损害本发明效果的范围内进一步含有其他成分。作为其他成分的例子,可以举出增强剂、软化剂、硫化剂、硫化促进剂、硫化助剂、加工助剂、硅烷偶联剂、以及乙烯-α-烯烃系共聚物以外的橡胶成分。
作为增强剂,例如可以举出SRF、GPF、FEF、MAF、ISAF、SAF、FT、MT等各种炭黑、碳酸钙、云母、硅酸镁、硅酸铝、木质素、氢氧化铝和氢氧化镁等。它们可以单独使用或组合使用。其中,这些之中,多孔粒子以及具有离子交换性的粒子被分类为成分(D)的添加粒子。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的增强剂的含量可以为200质量份以下或150质量份以下。
作为软化剂,可以举出加工油、润滑油、石蜡、液体石蜡等石蜡系油、环烷烃系油、石油沥青、凡士林、煤焦油沥青、蓖麻油、亚麻油、橡胶替代品(rubber Substitutes)、蜂蜡、蓖麻油酸等。它们可以单独使用或组合使用。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的软化剂的含量可以为100质量份以下或70质量份以下。
作为硫化剂,可以举出硫、硫系化合物和有机过氧化物等。硫化剂可以包含有机过氧化物。它们可以单独使用或组合使用。硫可以为粉末硫、沉降硫、胶体硫、表面处理硫或不溶性硫等。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的硫和硫系化合物的含量可以为0.01~10质量份或0.1~5质量份。
作为有机过氧化物,可以举出过氧化二枯基、2,5-二甲基-2,5-二(叔丁基过氧化)己烷、2,5-二甲基-2,5-二(苯甲酰过氧化)己烷、2,5-二甲基-2,5-二(叔丁基过氧化)-3-己炔、二叔丁基过氧化物、二叔丁基过氧化-3,3,5-三甲基环己烷、以及叔丁基过氧化氢等。有机过氧化物可以为选自过氧化二枯基、二叔丁基过氧化物、以及二叔丁基过氧化-3,3,5-三甲基环己烷中的至少1种化合物,也可以为过氧化二枯基。相对于乙烯-α-烯烃系共聚物橡胶100质量份,有机过氧化物的含量可以为0.1~15质量份或1~8质量份。
作为硫化促进剂,可以举出一硫化四甲基秋兰姆、二硫化四甲基秋兰姆、二硫化四乙基秋兰姆、二硫化四丁基秋兰姆、一硫化双五亚甲基秋兰姆、二硫化双五亚甲基秋兰姆、四硫化双五亚甲基秋兰姆、二硫化N,N’-二甲基-N,N’-二苯基秋兰姆、二硫化N,N’-双十八烷基-N,N’-二异丙基秋兰姆、N-环己基-2-苯并噻唑-次磺酰胺、N-氧二亚乙基-2-苯并噻唑-次磺酰胺、N,N-二异丙基-2-苯并噻唑次磺酰胺、2-巯基苯并噻唑、2-(2,4-二硝基苯基)巯基苯并噻唑、2-(2,6-二乙基-4-吗啉代硫基)苯并噻唑、二硫化二苯并噻唑、二苯胍、三苯胍、二邻甲苯胍、邻甲苯双胍、二苯胍-邻苯二甲酸酯、正丁醛苯胺、六亚甲基四胺、乙醛氨、2-巯基咪唑啉、对称二苯硫脲、二乙基硫脲、二丁基硫脲、三甲基硫脲、二邻甲苯基硫脲、二甲基二硫代氨基甲酸锌、二乙基硫代氨基甲酸锌、二正丁基二硫代氨基甲酸锌、乙基苯基二硫代氨基甲酸锌、丁基苯基二硫代氨基甲酸锌、二甲基二硫代氨基甲酸钠、二甲基二硫代氨基甲酸硒、二乙基二硫代氨基甲酸碲、二丁基黄原酸锌、以及亚乙基硫脲等。它们可以单独使用或组合使用。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的硫化促进剂的含量可以为0.05质量份以上且20质量份以下、或者0.1质量份以上且8质量份以下。
作为硫化助剂,可以举出三烯丙基异氰脲酸酯、N,N’-间苯撑双马来酰亚胺、甲基丙烯酸、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸异丙酯、甲基丙烯酸正丁酯、甲基丙烯酸异丁酯、甲基丙烯酸仲丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸-2-乙基己酯、甲基丙烯酸环己酯、甲基丙烯酸异癸酯、甲基丙烯酸月桂酯、甲基丙烯酸十三烷基酯、甲基丙烯酸硬脂酯、甲基丙烯酸-2-羟基乙酯、甲基丙烯酸羟丙酯、聚乙二醇单甲基丙烯酸酯、聚丙二醇单甲基丙烯酸酯、甲基丙烯酸-2-乙氧基乙酯、甲基丙烯酸四氢糠酯、甲基丙烯酸烯丙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸苄酯、甲基丙烯酸二甲基氨基乙酯、甲基丙烯酸二乙基氨基乙酯、甲基丙烯酰氧基乙基磷酸酯、1,4-丁二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、新戊二醇二甲基丙烯酸酯、1,6-己二醇二甲基丙烯酸酯、二乙二醇二甲基丙烯酸酯、三乙二醇二甲基丙烯酸酯、聚乙二醇二甲基丙烯酸酯、二丙二醇二甲基丙烯酸酯、聚丙二醇二甲基丙烯酸酯、三羟甲基乙烷三甲基丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、烯丙基缩水甘油醚、N-羟甲基甲基丙烯酰胺、2,2-双(4-甲基丙烯酰氧基聚乙氧基苯基)丙烷、甲基丙烯酸铝、甲基丙烯酸锌、甲基丙烯酸钙、甲基丙烯酸镁、3-氯-2-羟丙基甲基丙烯酸酯、氧化锌和氧化镁等。它们可以单独使用或组合使用。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的硫化助剂的含量可以为0.05质量份以上且15质量份以下、或者0.1质量份以上且8质量份以下。
作为加工助剂,例如可以举出油酸、棕榈酸和硬脂酸等脂肪酸;月桂酸锌、硬脂酸锌、硬脂酸钡和硬脂酸钙等脂肪酸金属盐;脂肪酸酯;乙二醇和聚乙二醇等二醇。它们可以单独使用或组合使用。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的加工助剂的含量可以为0.2质量份以上且10质量份以下、或者0.3质量份以上且8质量份以下。
作为硅烷偶联剂,可以举出硅烷系硅烷偶联剂、乙烯基系硅烷偶联剂、甲基丙烯酸系硅烷偶联剂、环氧系硅烷偶联剂、巯基系硅烷偶联剂、硫系硅烷偶联剂、氨基系硅烷偶联剂、脲基系硅烷偶联剂、以及异氰酸酯系硅烷偶联剂等。它们可以单独使用或组合使用。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的硅烷偶联剂的含量可以为0.1质量份以上且10质量份以下、或者0.5质量份以上且8质量份以下。
作为乙烯-α-烯烃系共聚物橡胶以外的橡胶成分,例如可以举出天然橡胶、异戊二烯橡胶、丁二烯橡胶、丁苯橡胶、丁基橡胶。相对于乙烯-α-烯烃系共聚物橡胶100质量份,橡胶组合物中的乙烯-α-烯烃系共聚物橡胶以外的橡胶成分的含量可以为10质量份以上且40质量份以下、或者15质量份以上且30质量份以下。
本实施方式的橡胶组合物能够为不含有由卤素系化合物构成的阻燃剂的无卤素组合物。若利用无卤素的阻燃剂表现出高度的阻燃性,则具有特别容易产生模具污染的倾向,但本实施方式的橡胶组合物即便为无卤素,也能够表现出高度的阻燃性和被抑制的模具污染这两者。
橡胶组合物例如可以通过对包含乙烯-α-烯烃系共聚物橡胶和其他成分的混合物进行混炼而得到。混炼可以使用搅拌机、捏合机和双螺杆挤出机等密闭式混炼机来进行。混炼能够进行至各成分被均匀地混合为止。混炼时间可以为1分钟以上且60分钟以下。混炼温度可以为40℃以上且200℃以下。
橡胶成型体
一个实施方式的橡胶成型体包含上述实施方式的橡胶组合物和/或其硫化物。图1是示出橡胶成型体的一个实施方式的截面图。图1中例示的橡胶成型体1例如可以通过下述方法来制造,该方法包括在模具内将橡胶组合物加热成型。制造橡胶成型体的方法可以包括:在模具内将橡胶组合物加热成型而形成橡胶成型体;以及对橡胶组合物进行硫化。可以一边加热形成橡胶成型体一边对橡胶组合物进行硫化,也可以在形成橡胶成型体后,对形成了橡胶成型体的橡胶组合物进行硫化。
对于橡胶组合物,例如利用注射成型机、压缩成型机、热空气硫化装置等成型机,一边加热至120℃以上且250℃以下、或者以1分钟以上且60分钟以下加热至140℃以上且220℃以下,一边在模具内成型,由此能够得到经硫化的橡胶成型体。
橡胶成型体可以作为阻燃性橡胶而发挥功能。该橡胶成型体例如能够用于阻燃电线、阻燃垫片、阻燃电装部件等各种构件。
实施例
以下,基于实施例对本发明进行更具体的说明。但是,本发明并不限定于此。
1.共聚物橡胶的评价方法
(1)乙烯单元的含量和丙烯单元的含量
将共聚物橡胶用热压机进行成型,制作出厚度约0.1mm的膜。利用红外分光光度计(日本分光公司制、IR-810)测定该膜的红外吸收谱图。根据所得到的红外吸收谱图,依照参考文献(基于红外吸收谱图的聚乙烯的表征高山、宇佐美等著或者Die MakromolekulareChemie,177,461(1976)Mc Rae,M.A.,MaddamS,W.F.等著)中记载的方法,求出乙烯单元的含量和丙烯单元的含量。
(2)碘值
依照“JIS K0070-1992 6.碘值”,将碘值不同的三种乙烯-丙烯-5-亚乙基-2-降冰片烯共聚物橡胶分别用热压机成型,制作出厚度约0.2mm的膜。利用红外分光光度计(日本分光株式会社制、IR-700)测定各膜的红外吸收谱图。根据所得到的红外吸收谱图,求出各膜的来自5-亚乙基-2-降冰片烯的峰(1686cm-1的吸收峰)和基峰(1664~1674cm-1的吸收峰)的透射率,根据下述式(I)计算出IR指数。A为基峰的透射率,B为来自5-亚乙基-2-降冰片烯的峰的透射率,D(mm)为膜的厚度。
IR指数=Log(A/B)/D…式(I)
根据IR指数和上述已知的碘值,得到下述式(II)所示的碘值的标准曲线。
碘值=α×IR指数+β…式(II)
式(II)中的α和β分别为常数。
(3)分子量分布
利用凝胶渗透色谱(GPC)法,以下述条件测定共聚物橡胶的重均分子量(Mw)和数均分子量(Mn)的标准聚苯乙烯换算值。
·GPC装置:东曹株式会社制造、商品名HLC-8121GPC/HT
·柱:东曹株式会社制造、商品名TSKgel GMHHR-H(S)HT
·分子量标准物质:分子量为500以上且20,000,000以下的聚苯乙烯
·洗脱溶剂流速:1.0mL/min
·试样浓度:1mg/mL
·测定温度:140℃
·洗脱溶剂:邻二氯苯
·注入量:500μL
·检测器:差示折射计
2.橡胶组合物的制备及其评价
实施例1(橡胶组合物的制备)
将作为成分(A)的乙烯-丙烯-5-亚乙基-2-降冰片烯共聚物橡胶100质量份、作为成分(B)的含有磷原子和氮原子的磷系阻燃剂(株式会社ADEKA制造、商品名“ADK STAB FP-2100JC”)140质量份、作为成分(C)的热膨胀性石墨(AIR WATER INC.制造、商品名“MZ-260”)20质量份、作为成分(D)的多孔二氧化硅粒子(Tosoh Silica Corporation制造、商品名“Nipsil VN3”)1.5质量份、以及作为其他成分的下述添加剂用起始温度调整为70℃的1700mL的班伯里密炼机(神户制钢公司制造)以80rpm的转子转速混炼4分钟。
其他成分:
·季戊四醇(广荣化学工业株式会社制造):1质量份
·炭黑(ASAHI CARBON CO.,LTD.制造、商品名“旭#60H”):40质量份
·石蜡油(Cosmo石油株式会社制造、商品名“Cosmo SR700”):35质量份
·氧化锌(正同化学工业公司制造、商品名“氧化锌2种”):5质量份
·硬脂酸(新日本理化公司制造、商品名“硬脂酸50S”):1质量份
利用上述方法对作为成分(A)的共聚物橡胶而使用的乙烯-丙烯-5-亚乙基-2-降冰片烯共聚物橡胶进行评价,结果具有以下的特性。
·乙烯单元的含量:65%
·丙烯单元的含量:31%
·碘值:11
·分子量分布:2.4
将所得到的混炼物343.5质量份、二正丁基二硫代氨基甲酸锌(Rhein Chemie公司制造商品名Rhenogran ZDBC-80)2.5质量份、二硫化四甲基秋兰姆(Rhein Chemie公司制造商品名Rhenogran TMTD-80)0.63质量份、四硫化双五亚甲基秋兰姆(Rhein Chemie公司制造商品名Rhenogran DPTT-70)0.71质量份、2-巯基苯并噻唑(Rhein Chemie公司制造商品名Rhenogran MBT-80)1.25质量份、以及硫1.5质量份用8英寸的开炼辊(KANSAI ROLL Co.,Ltd.制造)以40℃的辊温度进行混炼,得到橡胶组合物。
(橡胶成型体的制造)
将所得到的橡胶组合物用100吨压力机(商品名:PSF-B010、KANSAI ROLL Co.,Ltd.制造)以170℃的设定温度一边加热一边在模具内压缩20分钟,从而一边硫化一边成型,制作出厚度2mm的硫化片。成型后,将硫化片从模具中取出。关于橡胶组合物的模具污染性,将通过目视实质上未确认到模具残存有附着物的情况评价为“良”,将确认到附着物残存的情况评价为“不良”。
(橡胶成型体的评价)
通过基于UL-94(垂直法)的阻燃性试验(依照UL SUBJECT 94(UnderwriterLaboratories Incorporated)的“设备的部件用塑料材料的燃烧试验”中规定的垂直燃烧试验),对所得到的硫化片的阻燃性进行评价。试验片的形状为长度125.0mm、宽度13.0mm、厚度2.0mm(2/25英寸)。
依照JIS K 7201-2测定所得到的硫化片的氧指数。试验片的形状为长度120.0mm、宽度6.5mm、厚度2.0mm。
实施例2~8、比较例1~5
如表1或表2所示地变更各成分的混配量,除此以外与实施例1同样地制备橡胶组合物并进行其评价。实施例6中使用的水滑石粒子为协和化学工业株式会社制造的“DHT-4A”(商品名)。
表1和表2示出实施例、比较例中的橡胶组合物的混配比、以及评价结果。表中的混配比为质量份。
[表1]
[表2]
可确认到:实施例的橡胶组合物均具有高阻燃性,并且在模具污染性的方面也优异。缺少包含磷原子和氮原子的阻燃剂或膨胀性石墨的比较例1、2的橡胶组合物、以及成分(D)的添加粒子的量超过15质量份的比较例5的橡胶组合物在模具污染性的方面优异,但阻燃性不充分。缺少成分(D)的添加粒子的比较例3、4的橡胶组合物尽管显示出高阻燃性,但在成型时发生了模具污染。
附图标记说明
1…橡胶成型体。
Claims (5)
1.一种橡胶组合物,其含有:
(A)包含乙烯单元和碳原子数为3以上的α-烯烃单元的乙烯-α-烯烃系共聚物橡胶;
(B)包含磷原子和氮原子的阻燃剂;
(C)热膨胀性石墨;以及
(D)作为多孔粒子或具有离子交换性的粒子的添加粒子,
相对于所述乙烯-α-烯烃系共聚物橡胶100质量份,所述阻燃剂的含量为50质量份~250质量份,所述添加粒子的含量为15质量份以下。
2.根据权利要求1所述的橡胶组合物,其中,相对于所述乙烯-α-烯烃系共聚物橡胶100质量份,所述添加粒子的含量为5质量份以下。
3.根据权利要求1或2所述的橡胶组合物,其中,所述乙烯-α-烯烃系共聚物橡胶包含乙烯-α-烯烃-非共轭多烯共聚物橡胶,所述乙烯-α-烯烃-非共轭多烯共聚物橡胶含有乙烯单元、碳原子数为3以上的α-烯烃单元和非共轭多烯单元。
4.一种橡胶成型体,其包含权利要求1~3中任一项所述的橡胶组合物和/或其硫化物。
5.一种橡胶成型体的制造方法,其包括在模具内将权利要求1~3中任一项所述的橡胶组合物加热成型。
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