CN1026239C - 乙丙橡胶/聚烯烃热塑性弹性体及制备方法 - Google Patents

乙丙橡胶/聚烯烃热塑性弹性体及制备方法 Download PDF

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CN1026239C
CN1026239C CN89100727A CN91109976A CN1026239C CN 1026239 C CN1026239 C CN 1026239C CN 89100727 A CN89100727 A CN 89100727A CN 91109976 A CN91109976 A CN 91109976A CN 1026239 C CN1026239 C CN 1026239C
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朱玉俊
马智茂
伍社毛
赵学兰
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BEIJING COLLEGE OF CHEMICAL TECHNOLOGY
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Abstract

一种全动态交联的乙丙橡胶/聚烯烃共混型热塑性弹性体及制备方法，它是由乙叉降冰片烯为第三单体的三元乙丙橡胶与聚烯烃、交联体系及配合剂和加工改性剂组成，采用酚醛树脂交联体系为乙丙橡胶的动态交联体系，油类、邻苯二甲酸酯和过氧化物的混合物为热塑性弹性体的加工改性剂。该材料具有流动性良好，硬度低，弹性高，耐疲劳；而且还可制得浅色和半透明的材料，可广泛用于汽车、建筑、医疗器械，电缆、包装和家用电器等领域。

Description

本发明涉及一种全动态交联的三元乙丙橡胶/聚烯烃共混型热塑性弹性体及制备方法。
乙丙橡胶/聚烯烃（EPDM/Polyolefin）热塑性弹性体是经全动态交联技术使橡胶相交联并以微细颗粒形式均匀分散在塑料中的共混物。该共混物可用热塑性塑料的加工方法进行加工，在较宽的温度范围内具有橡胶的弹性，是由乙丙橡胶与聚烯烃。交联体系及配合剂组成。
采用酚醛树脂作交联体系的乙丙橡胶/聚烯烃热塑性弹性体（美国专利US4311628），虽然比采用硫磺或二异丙苯过氧化物和二硫化四甲基秋兰姆作交联剂的热塑性弹性体（如美国专利US4130535和中国CN8510222）其流动性和硬度均有所改善。但由于它仅改换了交联剂，而加工助剂仍为一般传统配方，所公开的酚醛树脂为交联剂的热塑性弹性体，在橡胶/塑料重量比75～25/25～75范围内，材料最低硬度为71邵A，而要进一步提高橡胶/塑料重量比以降低硬度，其流动性则会受到一定影响。
本发明提出一种流动性良好，硬度低的新型乙丙橡胶/聚烯烃热塑性弹性体。在共混动态交联时，使用了含分子量较低的油类化合物和过氧化物作加工改性剂，使聚烯烃的分子量分布变宽，从而进一步提高了该热塑性弹性体中橡胶/塑料的重量比，使材料在低硬度下保持良好的流动性。
本发明所采用的橡胶是乙叉降冰片烯为第三单体的三元乙丙橡胶，塑料是聚烯烃（全同聚丙烯、高密度聚乙烯和低密度聚乙烯），熔融指数MI为0.6～13.0，其橡胶与塑料重量比为85/15至15/85。该热塑性弹性体的组分（重量份数）为：
乙丙橡胶    100份;
交联体系    2.8～37份;
防老剂    0.05～4份;
填充补强剂    5～200份;
填充油    0～250份;
加工改性剂    0.5～57份;
塑料    18～567份;
交联体系采用酚醛树脂交联体系，它可以是非溴化酚醛树脂为基体的交联体系（简称交联体系Ⅰ），也可是溴化酚醛树脂为基体的交联体系（简称交联体系Ⅱ）。交联体系Ⅰ是以叔丁基酚醛树脂或叔辛基酚醛树脂为交联剂、卤化物（例如：三氯化铁或氯化亚锡或氯化锌或氯磺化聚乙烯或氯丁橡胶或N-溴化琥珀酰亚胺或二苯基溴化四甲烷）为促进剂、硬脂酸为润滑剂组成。各组分（以橡胶为100重量份计）为：交联剂2～20份，促进剂0.3～18份，润滑剂0.5～5份。交联体系Ⅱ是以溴化叔辛基酚醛树脂（含溴量7～15%）为交联剂、卤化物（同上）为促进剂、氧化锌为活性剂、硬脂酸为润滑剂组成。各组分（以橡胶为100份计）为：交联剂5～20份，促进剂0.3～12份，活性剂1～10份，润滑剂0.5～5份。
本发明的热塑性弹性体用2，2，4-三甲基-1，2-二氢喹啉聚合物（防RD）作防老剂，以炭黑、白炭黑和透明白炭黑分别作为黑色、浅色和半透明热塑性弹性体中乙丙橡胶的填充补强剂，同时在黑色和浅色材料中还可加入滑石粉、活性陶土 和二氧化钛等填充补强剂。以高级芳烃油、环烷油和液体石蜡组成乙丙橡胶的填充油。以白油、机油和液体石蜡、邻苯二甲酸酯和过氧化二异丙苯组成的混合物为热塑性弹性体的加工改性剂，各组分重量百分比为：白油5～30%，机油5～30%，液体石油5～30%，邻苯二甲酸酯（邻苯二甲酸酯二丁脂或邻苯二甲酸酯二异辛酯）2.5～19%，过氧化二异丙苯0.07～15%。
本发明提出的热塑性弹性体可用一步法或两步法制得，两步法制得的材料性能更好，两步法是在密炼机或开放式炼胶机上加入前述本发明之组分的乙丙橡胶和交联体系及防老剂、填充补强剂、填充油等配合剂制得母胶，再在密炼机或双螺杆挤出机或开放式炼胶机上将母胶与聚烯烃进行动态交联，聚烯烃的加入量与母胶中含乙丙橡胶的重量之比为15/85～85/15。本发明所提出的热塑性弹性体的制备方法是：制母胶时，为使交联体系和配合剂在橡胶中分散均匀，又不至于使橡胶焦烧，因此制备母胶操作温度为40～95℃，出料温度为70～95℃;共混动态交联时，先将聚烯烃在高于其熔融温度10～25℃（聚丙烯为170～185℃，聚乙烯为135～150℃）条件下进行塑化，再与母胶在170～240℃温度下进行动态交联3～40分钟，在动态交联结束前2～5分钟加入加工改性剂，以使该热塑性弹性体具备良好的流动性。
本发明所提出的热塑性弹性体的主要性能如下：
物机性能：
硬度（邵氏）65A～45D，
200%定伸强度3.5～20.0MPa，
抗张强度6.0～27.0MPa，
撕裂强度20～100KN/m，
扯断伸长率250～500%，
永久变形20～80%，
长期使用温度-30～135℃，
短期使用温度可达150℃
135℃老化168小时的老化系数0.85～1.04;
流变特性：
当剪切速率≥200（S-1）时，该热塑性弹性体的流动粘度与聚丙烯（MI＝0.8）相当，挤出物表面光滑，口型膨胀率≤25%;
耐疲劳性：
当硬度（邵氏）≤86A时，该热塑性弹性体材料的不破裂的动态弯曲疲劳次数≥30万;
本发明与其它同类热塑性弹性体材料相比具有以下优点：流动性良好，硬度低，弹性高，耐疲劳;而且还可制得浅色和半透明的材料。可广泛用于汽车、建筑、医疗器械，电缆、包装和家用电器等领域。
表（1）、表（2）和表（3）为本发明实施例的配方及性能。表（1）所示A、C和D组为以非溴化酚醛树脂为基体的交联体系的配方例子，B和E为以溴化酚醛树脂为基体的交联体系的配方例子。
实施例1：
乙丙橡胶母胶的制备：按表（1）的配方A的组分要求在密炼机加乙丙橡胶及其交联体系和配合剂，操作温度为40～95℃，出料温度为70～95℃，操作时间为5分钟;
乙丙橡胶与聚烯烃共混动态交联：将密炼机升温至170～185℃，按表（2）配方1的要求投入聚丙烯塑化，后将乙丙橡胶母胶加入进行共混和动态交联，在温度180～240℃中操作5分钟，最后加入加工改性剂后2分钟出料，由开放式塑炼机（温度为180～200℃）压片，待冷却后由切粒机切粒装袋，性能见表（3）的配方1。
实施例2：
乙丙橡胶母胶的制备：按表（1）的配方B的组分要求在密炼机加乙丙橡胶及其交联体系和配合剂，操作温度和时间同实施例1;
乙丙橡胶与聚烯烃共混动态交联：将密炼机升温至135～150℃，按表（2）配方2的要求投入聚乙烯塑化，之后的操作同实施例1，性能见表（3）的配方2。
实施例3：
乙丙橡胶母胶的制备：按表（1）的配方C的组分要求在密炼机加乙丙橡胶及其交联体系和配合剂，操作温度时间同实施例1;
乙丙橡胶与聚烯烃共混动态交联：将密炼机升温至170～185℃，按表（2）配方3的要求投入聚丙烯塑化，之后的操作同实施例1，性能见表（3）的配方3。本实施例所得到的为半透明的热塑性弹性体。
实施例4：
乙丙橡胶母胶的制备：按表（1）的配方D的组分要求在密炼机加乙丙橡胶及其交联体系和配合剂，操作温度时间同实施例1;
乙丙橡胶与聚烯烃共混动态交联：将密炼机升温至170～185℃，按表（2）配方4的要求投入聚丙烯塑化，之后的操作同实施例1，性能见表（3）的配方4。
实施例5：
乙丙橡胶母胶的制备：在开放式炼胶机中按表（1）的配方E加入乙丙橡胶及其交联体系和配合剂，操作温度为40～95℃，出料温度为70～95℃，操作时间为10分钟。
乙丙橡胶与聚乙烯动态交联：将开放式炼胶机升温至135～150℃，投入聚乙烯塑化，按表（2）的配方5加入母胶进行共混和动态交联，在温度180～220℃下操作22分钟，最后加入加工改性剂，2～5分钟后出片，冷却后由切粒机切粒装袋，性能见表（3）的配方5。
实施例6：
加工改性剂是由白油、机油和液体石蜡、邻苯二甲酸酯和过氧化二异丙苯组成的混合物，各组分重量百分比为：
白油    5～30%;
机油    5～30%;
液体石蜡    5～30%;
邻苯二甲酸二丁脂    2.5～19%;
过氧化二异丙苯    0.07～15%;
表（1）母胶的配方（重量份数）
组成    配方号    A    B    C    D    E
乙丙橡胶    100    100    100    100    100
叔丁（辛）基酚醛树脂    10    5    16
三氯化铁    4
氯化亚锡    2
交    N-溴化琥珀酰亚胺    3
联    氯磺化聚乙烯    8
体    氯丁橡胶    15
系    硬脂酸    3    2    2    1    0.5
氧化锌    6    1
溴化叔辛基酚醛树脂    16    6
防老剂（防RD）    4    2    0.5    1    1
炭黑    42    15
填    白炭黑    44    18
充    透明白炭黑    50
补    滑石粉    33    12    76
强    活性陶土    80
剂    钛白粉    12    6
填    高级芳烃油    80    120    5    30
充    环烷油    45    75    40    15
油    液体石蜡    5    80    15    10
表（2）热塑性弹性体的配方（重量份数）
组成    配方号    1    2    3    4    5
橡胶/塑料    80/20    70/30    60/40    40/60    25/75
母胶A    261
母胶B    334
母胶C    153
母胶D    87
母胶E    60
聚丙烯    20    40    60
聚乙烯    30    75
加工改性剂    6    8    5    1    4
表（3）热塑性弹性体的性能
性能    配方号    1    2    3    4    5
硬度（邵氏）    67A    75A    82A    93A    47D
300%定伸强度（MPa）    5.5    8.6    9.5    12.6    18.9
物    扯断强度（MPa）    6.3    10.0    13.2    16.6    25.7
理    扯断伸长率（%）    330    325    378    412    474
性    撕裂强度（KN/m）    20    28    34    68    97
能    永久形变（%）    11    20    35    41    74
弯曲疲劳次数（万）    ≥30    ≥30    ≥30    -    -
耐
热空气老化系数
热    0.86    0.90    0.97    0.93    1.02
性    （135℃×168hr）
可    表面状态（φ5mm条）    ←    ←    表面光滑    →    →
挤    口型膨胀率（%）    7.0    8.4    10.2    14.1    20.0
性    挤出速率（cm/mln）    324    371    401    523    653

Claims (2)

1、一种全交联的乙丙橡胶/聚烯烃共混型热塑性弹性体，是由乙丙橡胶与聚烯烃、酚醛树脂交联体系和配合剂：防老剂、填充补强剂、填充油与加工改性剂组成，其特征在于：
(1)加工改性剂由油类、邻苯二甲酸酯和过氧化物组成，其组成为(重量百分比)：
白油            5～30%；
机油            5～30%；
液体石蜡        5～30%；
邻苯二甲酸酯    2.5～19%；
过氧化二异丙苯  0.07～15%；
(2)热塑性弹性体的组分为(重量份数)：
A)乙丙橡胶    100份；
B)交联体系    2.8～37份；
C)防老剂      0.05～4份；
D)填充补强剂  5～200份；
E)填充油      0～250份；
F)加工改性剂  0.5～57份；
G)聚烯烃      18～567份；
2、权利要求1所述的热塑性弹性体的制备方法，其特征在于：加工改性剂在热塑性弹性体动态交联结束前2～10分钟加入。
CN89100727A 1991-10-30 1991-10-30 乙丙橡胶/聚烯烃热塑性弹性体及制备方法 Expired - Fee Related CN1026239C (zh)

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