CN100519600C - 提高了抗刮性的聚烯烃及其制备方法 - Google Patents

提高了抗刮性的聚烯烃及其制备方法 Download PDF

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CN100519600C
CN100519600C CNB028292030A CN02829203A CN100519600C CN 100519600 C CN100519600 C CN 100519600C CN B028292030 A CNB028292030 A CN B028292030A CN 02829203 A CN02829203 A CN 02829203A CN 100519600 C CN100519600 C CN 100519600C
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E·哈根
U·托格森
G·罗哈泽克
A·艾弗兰德
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Abstract

本发明涉及改进了表面硬度和抗刮性的聚烯烃的制备方法，还涉及这种聚烯烃的用途。更具体地说，本发明涉及基于含双峰橡胶组合物的聚丙烯基质材料的聚烯烃制备方法。

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提高了抗刮性的聚烯烃及其制备方法
本发明涉及就抗刮性而言表面韧性得到提高的聚烯烃，及其制备制备方法。更具体地说，本发明涉及基于包括双峰橡胶组合物的聚丙烯基质材料的聚烯烃，以及上述聚烯烃的制备方法和作为矿物填充化合物原料的用途。
已知各种提高聚烯烃材料抗刮性的技术，即添加氧化硅材料。因此，JP1318051(Toray Silicone KK)公开了经过硅基填料改性的用于这种用途的聚烯烃。所述填料可用硅烷型化合物进行过表面处理。
JP1104637(Showa Denko KK)公开了聚丙烯基质料，其中已添加了氧化硅/氧化铝球状体和用羧酸或酸酐官能化的聚丙烯材料。
US 5484824公开了含乙烯丙烯橡胶的聚丙烯组合物，可用于制备汽车外部部件。
US 5308908涉及含乙烯/丙烯特定混合物和制造汽车保险杠用的其他烯烃共聚物的聚丙烯树脂组合物。
本申请人最近申请的EP-0804503揭示，将官能化聚丙烯材料和无定形脂肪酸酰胺改性的硅胶掺进具有一定矿物含量的聚烯烃材料中时，可明显提高材料的抗刮性，同时保持材料的冲击强度和热形状稳定性(HDTA)。
虽然上述材料表现出良好的抗刮性，但是这些材料是基于相当贵的填料系统，即经过表面处理的填料，由于价格高而导致难以加入市场。
在没有用任何改性组分如HDPE、增滑剂，高颜料淀积、特定滑石品质下，类似改性R-TPO’s的传统基质和高结晶度多相共聚物显示出有限的抗刮性，因此限制了这种材料在不同应用例如汽车内部、电器等抗刮性是重要性能的场合应用的可能性。
因此，需要在合理成本下表现出优异抗刮性的聚合物材料。
鉴于这种状况，本发明的发明者进行了深入细致的研究，发现：以下因素对抗刮性起到了积极作用：
—在聚丙烯基质中应含有两种Mw(IV)差别很大的橡胶组分和
—低IV橡胶必须是富含乙烯的。
运用该原理，富含乙烯的的橡胶颗粒更易于移向任何模塑制品的表面层。与富含丙烯的橡胶相比，富含乙烯的橡胶包含部分结晶聚乙烯，更均匀分布在靠近表面处，使得该表面具有更大的刚性/硬度，从而提高了抗刮伤破坏的能力。
如果需要，可以进行随后的混合工序，不需要贵的处理过的填料或过量贵的弹性体，仍能得到高抗刮性和需要的机械性能的组合。
还发现加入增滑剂如芥酸酰胺(erucamide)也能提高抗刮性。
因此，在第一个方面，本发明涉及带有双峰橡胶的聚丙烯聚合物组合物的制备方法，该方法包括：
i)在至少一个淤浆反应器中加入丙烯，在聚合催化剂存在下在所述至少一个淤浆反应器中制备制备聚丙烯聚合物基质，
ii)将淤浆反应器产物转移到气相反应器(GPR)，
iii)在所述第一气相反应器中加入乙烯和丙烯的第一混合物，并在聚合催化剂存在下在所述第一气相反应器中制备聚合物基质中的第一乙烯/丙烯-共聚物，
iv)将第一气相反应器的产品移至第二气相反应器，并
v)在上述第二气相反应器中加入乙烯和丙烯的第二混合物，并在聚合催化剂存在下在所述第二气相反应器中制备聚合物基质中的第二乙烯/丙烯-共聚物，
vi)回收步骤v)所制备生的聚合物产物，用于进一步加工，
所述第一和第二乙烯/丙烯混合物具有不同组成比。
在较好的实施方案中，本发明涉及一种方法，其中，对所述第一种和第二种乙烯/丙烯混合物的组成比加以调整，以便在第一气相反应器中制备在丙烯聚合物基质中的富含丙烯的EPR橡胶，在第二气相反应器中制备富含乙烯的EPR橡胶。
在另一个较好的实施方案中，富含丙烯EPR橡胶的分子量高于所述富含乙烯EPR橡胶。
最初的聚丙烯聚合物基质最好在淤浆反应器中制备，而不是在气相反应器中制备，然后淤浆相反应的产物宜进行闪蒸，以除去未反应的单体和H2，并移入气相反应器，在那里进一步反应形成二元乙丙橡胶。
本发明的聚丙烯聚合物基质最好在至少一个淤浆反应器中制备。
合适的制备方法可以由本领域技术人员容易地决定，包括但不限于：
A.在至少一个淤浆反应器中制备聚丙烯聚合物基质，然后将闪蒸过的淤浆反应器产物送送入气相反应器，并在第一气相反应器(GPR)中制备基质中的第一乙烯/丙烯共聚物，将闪蒸过的第一气相反应器产物送送入第二气相反应器(GPR)，在第二气相反应器(GPR)中制备基质中的第二乙烯/丙烯共聚物。
B.如A的第一步骤所述，在至少一个淤浆反应器中制备聚丙烯聚合物基质，然后将闪蒸过的淤浆反应器产物送入气相反应器，然后在所述反应器(GPR)中制备基质中的第一乙烯/丙烯共聚物，对该气相反应器产物进行闪蒸并将GPR产物重新通入气相反应器，在气相反应器中(GPR)制备基质中的第二乙烯/丙烯共聚物。
各种反应器的单体进料能适合于制备具有需要性能的聚合物，一般人员在预期本发明之后，能容易地确定单体量。
较好的，使用环管反应器作为所述淤浆反应器，虽然也可以使用其他类型的反应器如罐式反应器。按照另一个实施方案，所述淤浆相反应宜在两个淤浆反应器中进行，优选但不是必须，在两个环管反应器中进行。用这种方式，容易控制GPR的供料/加料速度。当在气相反应器中继续聚合时，可以确立基质丙烯聚合物的足够的供应量。
在淤浆反应器中，丙烯最好不仅用作聚合单体，而且还用作稀释剂。淤浆反应宜在环管反应器中进行，可通过将包含50-99.9wt％丙烯、达1wt％氢和催化剂体系的反应混合物送入至少一个淤浆聚合反应步骤，同时保持在低于75℃下烯烃聚合来进行。使用两个或更多个淤浆反应器时，它们最好是环管反应器，进料混合物最好与单一的淤浆反应器的进料混合物相同。
既可以在淤浆相反应器中也可在气相反应器中加入氢，以控制所制备的各聚合物的分子量。在烯烃聚合时使用氢是惯例，且易为专业人员所应用。
在第一气相反应器中，第一气相聚合步骤是这样进行的：加入丙烯和乙烯单体，使得在形成的EPR范围内所得到的C2的量为39-74mol％间，较好为53-65mol％。如果在该步骤要使用氢的话，C2/H2的摩尔比应在0.01-0.1之间，以0.03-0.06为佳，0.05最好。
在第二气相反应器中，第二气相聚合步骤是这样进行的：加入丙烯和乙烯单体，使得在形成的EPR中最终的C2量范围为77-99.9mol％，最好为84-96mol％。如果在该工序要使用氢的话，C2/H2的摩尔比应在0.3-0.7之间，以0.4-0.6为佳，0.5最好。
本发明人发现：按照与前述相反的顺序进行GPR聚合反应，可得到相同的抗刮伤(SR)性结果。这一点证实了本发明的发明原理，即在聚合过程的不同阶段制备双峰橡胶的rTPO对获得需要的SR特性的来说是至关重要的。
淤浆相聚合可以在温度低于75℃，较好62-70℃，压力变化范围为30-60bar，较好30-50bar的条件下进行。较好在这样的条件下进行聚合，即在淤浆反应器中聚合20-90wt％，较好40-80wt％的聚合物。
较好在高于10bar的压力下，通过将反应混合物从淤浆相转移出来通过闪蒸单元，以除去未反应的单体和H2，进行气相聚合反应步骤。所用反应温度一般在60-115℃范围内，较好为70-90℃。反应器压力可高于5bar，较好在8-16bar范围，停留时间一般为0.1-0.5小时。
可以采用任何标准烯烃聚合催化剂达到聚合，这些催化剂为本领域技术人员所熟悉。优选的催化剂系统包括普通的有规立构Ziegler-Natta催化剂、茂金属催化剂和其他有机金属或配位催化剂。一种特别优选的催化剂系统是高产率的Ziegler-Natta催化剂，具有催化剂组分、共催化剂组分、任选的外供体。因此催化剂系统包含钛化物和载于活化二氯化镁上的电子供体化合物、作为活化剂的三烷基铝化合物和电子供体化合物。
另一种优选的催化剂系统为茂金属催化剂，具有产生高立体选择性的桥连结构，该催化剂作为活性络合物被浸渍在载体上。
例如，在FI专利88047、EP 491566和WO 98/12234中描述了合适的催化剂系统，参考结合于此。
本发明的多相共聚物中基质组分的量为多相聚合物重量的20-90％，较好60-90％，最好65-70％。在乙烯含量低的GPR聚合步骤中制备的弹性共聚物量可以是多相聚合物重量的10-30％，较好15-25％，最好18-22％。在富含乙烯的GPR聚合步骤中制备的弹性共聚物量可以是多相聚合物重量的5-20％，较好10-15％，最好12-15％。弹性体组分可以包含95-5wt％，较好95-20wt％的结晶相和5-95wt％，较好5-80wt％的无定形相。
多相共聚物的二甲苯可溶级分(XS)较好是基质组分重量的3-35％、最好6-20％。
丙烯聚合物基质也可以包含任何合适单体比的丙烯、乙烯和如果需要的任选其他α-烯烃，产生无定形或半结晶/无定形弹性共聚物。弹性组分最好只包含乙烯和丙烯共聚物。
聚合物组合物可以与矿物材料混合，进一步提高机械性能。适用于本发明聚烯烃合金中的矿物为细粉矿物，并经过表面处理，例如用一种或多种传统上用来对滑石进行表面处理的氨基硅烷加以硅烷化。最适合在合金中使用的矿物为钙硅石、高岭土、云母、碳酸钙和滑石，特别是滑石。矿物的平均粒径D50较好为0.5-10μm，1-6μ
m更好。
本发明聚合物组合物还可以包含目前本领域制备常用的和在“Plastics AdditivesHangbook”，Hanser Verlag Munich 2001中例举的添加剂和填料。
本发明聚合物组合物还可以包含可能对抗刮性有好处的增滑剂。这样的增滑剂可选自脂肪酸酰胺，如芥酸酰胺、油酸酰胺和高分子量聚硅氧烷。
目标转化技术为，但不限定于注塑。
按照本发明方法制备混合聚合物组合物可用来替代ABS或ABS/PC-制电器应用的部件，在该用途中抗刮性是重要的性能，汽车内部部件和外部部件具体地说，为挡泥板、车门金属包层、控制台、保险杠，这些地方需要改善SR性能。
本发明因此还涉及用本发明组合物制备制造的那些部件。
实施例
用一个淤浆环管反应器和两个气相反应器组合，按照本发明制备聚丙烯共聚物。
粉末状的反应器产物本身具有非常好的抗刮性，可用于诸如机械性能足够好之类的应用。汽车和电器方面的许多用途对刚性的要求较高，因此矿物增强措施是必要的。为达到矿物材料在PP中的分布情况良好的目的，需要混合步骤。有鉴于此，在混合工序使用以下添加剂。
75.9％反应器产物
0.1％催化剂
0.2％Irganox B225
0.3％GMS
0.5％芥酸酰胺
3.0％黑灰色MB
20％Talcum Luzenac A20(D50 20μm)
所用的共混挤压机为Prism TSE 24HC，双螺杆挤压机，(螺杆直径D＝24mm，总长＝40D)。可以参见挤出机图。
通过主加料器加入聚合物粉末和添加剂，通过副加料器添加20％滑石。在1-10区和模头的设定温度如下：
20，200，205，210，215，215，215，215，210和210℃，为PP共混用标准设定值。
为在实施例1-5进行机械试验，使用注塑试验棒，80×10×4mm和60×60×3mm。这些试验棒是在Battenfeld 460注塑机上采用PP用标准温度设定制备的。
刮伤试验用造粒试验盘的制造方法是：在预造粒磨具中用由GM定义称作N111(细磨粒)和N127(粗磨粒)的颗粒进行注塑。此外，模塑一个非造粒的盘，作刮伤深度研究之用。
在测试和聚合物合成中采用下列方法：
按照ISO 1133，在2.16kg负荷和230℃下，测定熔体流动速率(MFR)。
按照ISO 572-2(十字头速度＝50mm/min)，测定拉伸强度(屈服时的拉伸应力)。
按照ISO 572-2(十字头速度＝1mm/min)，测定拉伸模量。
按照ISO 178测定弯曲模量。
按照ISO 179/leA，测定卡毕冲击强度、切口冲击强度。
按照DIN 75 201 B测定成雾。
按照VDA 277测定碳发射。
按以下具体说明测定抗刮性。
抗刮性试验方法
由于没有统一的抗刮性定义，本发明者找到了一种一致适用的试验方法。基本上，刮伤理解为材料因短暂机械应力的作用而造成材料表面持续形变或磨损。所述的刮伤主要取决于填料的类型和用量、表面构造、压杆的形状和作用力，聚合物的表面硬度和刮痕底部的光洁度，所述刮伤必须进行检查再可见性(re visibility)(光散射)，形变的面积/大小和深度。本发明人发现，用专用试验仪器可以获得可靠和可比较的结果。
所述方法是建立在使用GM的方法基础上的，GM(GME 60280)带有刮伤装置(交叉开口切割器型号420p，Erichsen制备制造)，用于有不同颗粒(N111----→细颗粒/N127----→粗颗粒)的试样表面上切出交叉开口。该测量仪装有钢球尖头(0.5-3.0mm)。在用简单机构产生切割速度(通常为1000m/min)的同时切割力可在1到50N范围内调节。实施例中所用的标准条件是建立在5N力、1.0mm尖头和1000m/min切割速度基础上的。
为更客观地评价划痕，选择这种方法来代替传统的Erichsen测试仪(318型)，因为避免了进行试验人员的影响。
用光谱分析仪测定ΔL(dL)值的方法进行刮伤评价。这一测试值相当于处理过的和未处理过的聚合物表面亮度差。
ΔL>4：强刮伤可见性ΔL<1：在该值以下刮伤的可见性明显降低。
除扫描电子显微镜和激光器外，还使用共焦显微镜来检查刮伤的外形和深度。
实施例1-5
在一个环管反应器中进行PP-基质聚合。第一步骤，在70℃的液态丙烯中制备生基质。经过要求的聚合时间，慢慢地将压力降低到10.5bar，对基质产品进行闪蒸后，在气相反应器中继续进行聚合。在气相，半结晶和无定形共聚物在80℃聚合。
按照标准方法制备使用的催化剂，催化剂活性为40kg PP/g催化剂小时。聚合反应条件和聚合物性能列于表1。
试验结果
 
批次 IV裂口GPR1/GPR2(GPR2＝总量) C2 mol％GPR1/GPR2(GPR2＝总量) 橡胶总含量(％) MER230℃粒料 弯曲模量MPa 卡毕强度(+)23℃kJ/m<sup>2</sup> 卡毕强度(-)20℃kJ/m<sup>2</sup>
1 1.63/3.22 12.2/21.1 28.9 9.8 79860.2 (PB)8.7 (B)
2 1.61/2.43 10.9/28.7 29.1 13.1 873 12.1(B) 6.0(B)
3 4.00/3.45 14.4/33.0 29.5 10.6 925 10.6(B) 5.6(B)
4 4.24/2.34 25.2/30.1 29.0 11.9 828 13.2(B) 6.1(B)
5 2.31/2.63 11.9/23.0 26.5 13.2 900 12.2(B) 6.2(B)
批号1到5的化合物与20％滑石(Luzanac A-20)和芥酸酰胺混合，试验样品的抗刮性已经过检验。
 
批号 SR，dLN111/N127 灰分％ MFR230℃粒料 弯曲模量MPa 卡毕强度(+)23℃kJ/m<sup>2</sup> 卡毕强度(-)20℃kJ/m<sup>2</sup>
1-1 1.9/3.2 20.4 10.4 1786 27.2(PB) 4.2(B)
1-2 3.3/4.5 20.3 9.6 1932 25.9(PB) 3.9(B)
2 1.9/2.9 19.3 11.6 1915 6.7(B) 2.4(B)
3 0.8/1.3 20 11.2 1911 9.1(HB) 2.3(B)
4 1.8/2.9 20.9 10.9 1852 7.5(HB) 2.4(B)
5 0.94/1.7 20.3 12 1870 10.0(HB) 2.6(B)
*)批号1-2是基于同样的PP料，但不含芥酸酰胺，结果表明在含有非优化EPR的PP中添加增滑剂SR可有额外的提高。
从上述发明人的研究结果中可以看出，当高C2含量与低分子量IV结合时可获得最佳抗刮性能。对批号3和5的试验结果进行比较可以看出，只要保持各步骤的C2摩尔比，不同GPR聚合反应顺序对获得需要的SR性来说并不是最至关重要的。
如果需要较高的抗冲击强度，应提高橡胶总含量，应区分GPR的分裂，以产生更多富含C3的橡胶。就高刚性而言，可以使用较细的滑石、强成核剂，而且应使C2的含量最大。
使用本发明方法，可以得到的这样的聚合物材料：其dL值较好小于4，使用增滑剂，尤其是芥酸酰胺时，该值得到进一步改善，更好低于2(dL<2)。

Claims (11)

1.一种有双峰橡胶的聚丙烯聚合物组合物的制备方法，所述方法包括以下步骤：
i)在至少一个淤浆反应器中加入丙烯，并在聚合催化剂存在下，在所述至少一个淤浆反应器中制备聚丙烯聚合物基质，
ii)将淤浆反应器产物移至第一气相反应器中，
iii)在所述第一气相反应器中加入乙烯和丙烯的第一混合物，并在聚合催化剂存在下，在所述第一气相反应器中制备聚合物基质中的第一乙烯/丙烯共聚物，
iv)将第一气相反应器产物移至第二气相反应器中，和
v)在所述第二气相反应器中加入乙烯和丙烯的第二混合物，并在聚合催化剂存在下，在所述第二气相反应器中制备聚合物基质中的第二乙烯/丙烯共聚物，
vi)回收由步骤v)制得的聚合物产物，以进一步加工，
所述第一和第二乙烯/丙烯混合物的组成比不同，调节所述第一和第二乙烯/丙烯混合物的组成比，以便在第一气相反应器中制备丙烯聚合物基质中的富含丙烯的EPR橡胶，在第二气相反应器中制备丙烯聚合物基质中的富含乙烯的EPR橡胶。
2.权利要求1所述的方法，其特征在于气相反应器中的聚合反应条件是这样的：在第一气相反应器中，通过加入乙烯和丙烯单体进行气相聚合反应步骤，使得在第一气相反应器中形成的EPR中乙烯的量在39-74mol％的范围内，在第二气相反应器中，通过加入乙烯和丙烯单体进行气相聚合反应步骤，使得在第二气相反应器中形成的EPR中乙烯的量在77-99.9mol％的范围内。
3.如权利要求2所述的方法，其特征在于在第一气相反应器中形成的EPR中乙烯的量在53-65mol％的范围内，在第二气相反应器中形成的EPR中乙烯的量在84-96mol％的范围内。
4.前述权利要求中任一项所述的方法，其特征在于在将聚合物产物转移到下一聚合步骤之前先进行闪蒸。
5.前述权利要求1-3中任一项所述的方法，其特征在于从步骤vi得到的聚合物产物经进一步处理，以与添加剂和/或填料混合。
6.聚合物产品，按照前述权利要求中任一项所述的方法获得，该聚合物产品是多相共聚物，它包含65-70重量％的聚丙烯聚合物基质、10-30重量％富含丙烯的EPR橡胶和5-20重量％富含乙烯的EPR橡胶。
7.权利要求6所述的聚合物产品，其特征在于所述产品还包含至少一种选自矿物、增滑剂和加工助剂的添加剂或填料。
8.权利要求6所述的聚合物产品，该产品的dL值小于4，所述dL值相当于处理过的和未处理过的聚合物表面的亮度差。
9.权利要求8所述的聚合物产品，其特征在于dL值小于2。
10.权利要求6-9中任一项所述的聚合物的用途，用于制造模塑制品。
11.模塑制品，包含权利要求6-9中任一项所述的聚合物。
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