CN105051100B - 矿物填充的聚丙烯组合物 - Google Patents
矿物填充的聚丙烯组合物 Download PDFInfo
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Abstract
本发明涉及用于生产模制品,例如用于汽车工业的成品零件的低密度聚丙烯组合物。
Description
技术领域
本发明涉及热塑性的聚丙烯组合物及其以滑石作为矿物填充物的填充组合物,用于生产表面光滑、加工性能良好和低密度的用于内部装饰和外部零件的模制品。
背景技术
通常,具有光滑的模印表面的制品用于内部设计,例如汽车或飞机以及外部汽车零件的装饰部件。汽车工业对成品零件实施严格的要求。低总量的二氧化碳排放、低雾化性、很少的气味以及具有良好抗刮擦性是用于内部装饰(例如仪表面板、门板和三角板装饰)的典型要求,所述内部装饰通常是注塑成型。
所述外部零件,包括缓冲器组件和如前端载波模块的结构模块,通常需要高性能填充的化合物。外部装饰,如侧面保护装饰、前围罩、轮口衬垫以及覆盖件,如摇板、主体侧嵌条或挡泥板,需要特定的性能与良好外观相结合。
US 6441094公开了包括具有不同熔体流率值(双峰基质)的两个聚合物馏分和通过乙烯的弹性共聚物形成的橡胶相的耐冲击性聚烯烃组合物。在US 6441094中的聚烯烃组合物呈现出加工性能与机械和光学性能的独特平衡且它们特别适合于注塑成型零件。
用于外部和内部装饰的材料需要提供灵活性组合性能,如精密的间隙公差、优越的抗刮擦性以及良好的油漆粘附性和加工性能。
由于它们的自由流动的特性,迄今,填充滑石的不同混合物已经用在这样的应用中。由于它们固有的低抗弯刚度,限制滑石加强的混合物的电势可用于模制精密的成品,例如汽车仪表盘。近来,希望使用保持高机械性能的低密度材料满足对轻型小客车-零件的增加的需求,以提高燃料效率但不损害安全和性能。已知的滑石填充的组合物以重量增加为代价提高填料量,提供了增强的刚度性能。减少滑石通常会使刚度降低,增加聚合组分的刚度可以补偿降低的刚度,但是这以收缩率为代价,从而对模具中的精密的间隙公差产生不利影响。
希望避免现有技术的缺点来设计一种用于模制品的新的低密度轻量的复合材料,其保有现有技术混合物的优点,尤其是它们的优异的自由流动性和收缩率以及冲击/刚度平衡。
发明内容
本发明组合物适用于传统模具,其“间隙公差”和“用具收缩率”可与现有技术中已知的较高密度组合物相媲美。因而,本发明组合物是在汽车领域有价值的普适型解决方案,其使用了具有经济优势和供应可靠性的现有模具。
因此,本发明的目的是一种具有密度小于1g/cm3的组合物,包括:
(A)15-60wt%,优选为20-30wt%的一种或多种丙烯基组分,所述丙烯基组分选自丙烯均聚物、丙烯共聚物或其组合,这样的第一丙烯基组分具有根据ISO 178测定的大于1500MPa,优选大于2000MPa的弯曲模量,和大于10,优选大于13的PI;
(B)20-50wt%,优选为35-45wt%的异相丙烯聚合物,其具有10-20g/10min的熔体流动速率,所述异相丙烯聚合物包括:
(B1)50-90wt%,优选为60-80wt%的结晶聚丙烯,优选地具有在室温下在二甲苯中小于5wt%的组分(B1)的溶解度,且进一步优选地具有大于50g/10min的熔体流动速率;
(B2)10-50wt%,优选为20-40wt%的乙烯与作为共聚单体的至少一种C3-C10α-烯烃(优选地丙烯作为共聚单体)的共聚物,该共聚物含有40-60wt%的乙烯,优选地具有在室温(25℃)下在二甲苯中大于70wt%的组分(B2)的溶解度;
(D)5-25wt%,优选为10-20wt%的乙烯基塑性体或弹性体,其具有硬度(邵氏A,ASTM D-2240)值等于或低于90点,优选为等于或低于85点,更优选为等于或低于80点,密度低于0.890g/cm3;
(E)0-20wt%,优选为1-15wt%,更优选为10-15wt%的滑石,优选为高纵横比滑石,优选为层状指数等于或大于2.8的滑石;
(C)0-10wt%,优选为1-10wt%,更优选为3-8wt%的高密度聚乙烯(HDPE)。
该组合物的各个组分的百分比量的总和等于100%,优选地该组合物在常规聚合载体(例如标准聚丙烯均聚物)中包括0-10wt%的添加剂和颜料的预混合料。
该组合物的各个组分的百分比量的总和等于100%,优选地该组合物在常规聚合载体(例如标准聚丙烯均聚物)中包括0-10wt%的添加剂和颜料的预混合料。
第一丙烯基组分(A)适当地可以是含有多达5wt%的乙烯和可选择地一个或多个C4-C10α-烯烃的丙烯均聚物或共聚物。可用作共聚单体的C4-C10α-烯烃的实例子包括1-丁烯、1-戊烯、1-己烯、4-甲基-1-戊烯和1-辛烯,其中特别优选的是1-丁烯。
优选地,所述组分(A)的MFR(230℃,2.16kg)值是10-150g/10min,更优选地为20-50g/10min。
同样优选地,所述组分(A)在室温(25℃)下二甲苯可溶部分的含量小于7wt%,优选地小于5wt%,甚至更优选地小于3wt%。
所述组分(A)可以根据EP0573862中所述的方法且在齐格勒纳塔催化剂的存在下而获得。
所述组分(B)可以适当地通过序列聚合制备,所述序列聚合包括至少两个序列步骤,其中在单独的序列步骤中制备出组分(B1)和(B2),每一步中的操作都在前一步骤中形成的聚合物和使用的催化剂的存在下进行。组分(B)是由丙烯聚合物基质和乙烯-α-烯烃共聚物橡胶组成的异相共聚物,乙烯-α-烯烃共聚物橡胶优选地是乙烯-丙烯共聚物橡胶组分(EPR)。
在第二丙烯基组分(B)内,该组分(B1)优选地是在25℃下不溶于二甲苯的至少为98wt%的结晶丙烯均聚物。结晶组分(B1)优选地具有高于70g/10min的熔体流动速率。
在第二丙烯基的组分(B)内,组分(B2)优选地是乙烯-丙烯共聚物,所述乙烯-丙烯共聚物含有在室温(25℃)下可溶于二甲苯的45-55wt%,优选地至少80wt%的乙烯。合适作为组分(B)的聚合物组合物可以用催化剂组分制备,所述催化剂组分诸如为在EP0728769(实施例5)中公开的催化剂组分,其中烷基-烷氧基硅烷作为外给体。
根据本发明,通过硫化作用交联组分(A)和(B)既不必要也不需要。
通常,适合用于本发明的组合物中的乙烯基塑性体(D)是乙烯与C3-C10α-烯烃的共聚物,该共聚物含有衍生自C3-C10α-烯烃的至少20wt%、优选地为20-50wt%的单元(碳-13核磁共振分析)。
乙烯基塑性体(D)的密度(根据ASTM D-792测量)低于0.89g/cm3,优选地低于0.87g/cm3。
乙烯基塑性体(D)的优选实例是:
具有至衍生自1-辛烯的20-45wt%的单元(碳-13核磁共振分析)的乙烯与1-辛烯的共聚物;
具有至衍生自1-丁烯的20-40wt%的单元(碳-13核磁共振分析)的乙烯与1-丁烯的共聚物;
通常,适合用于本发明的组合物中的滑石(E)是具有范围为从(D50)0.1到20微米(μm)的平均粒度(Sedigraph ISO 13317-3)的颗粒形式。用于本发明的组合物中特别优选使用的是具有等于或高于2.8的层状指数的高纵横比滑石。层状指数表征颗粒的形状,并且更具体地表征颗粒的平整度(大的尺寸/厚度)。可由一方面粉末的颗粒的平均尺寸的值和另一方面平均直径D50的值之间的差值检测出层状指数,该差值涉及平均直径D50,所述一方面粉末的颗粒的平均尺寸的值通过使用湿法(标准的法国标准化协会(AFNOR)NFX11-666)的马尔文激光衍射粒径测量获得,所述另一方面平均直径D50的值通过使用“Sedigraph”(标准的法国标准化协会(AFNOR)X11-683)的沉降测量获得。参考文章“G.BAUDET和J.P.RONA,Ind.Min.Mines et Carr.Les techn.1990年6月、7月,55-61页”,该文章显示该指数与颗粒的最大尺寸与颗粒的最小尺寸的平均比值有关。“高层数”理解为是指层状指数高并且特别大于2.8、优选地等于或高于4的粉末。
根据一个实施例,当本发明的组合物包括组分(C)时,即这些组合物包括大量高密度聚乙烯(HDPE),它们显示其抗刮擦性得到显著提高。
根据另一实施例,通过掺入少量的抗刮擦添加剂,抗刮擦性也得到改善。在本领域中公知,在本发明的组合物中可以使用的抗刮擦添加剂具有导致更少刮擦可见性的润滑作用。这样的化合物的实例为芥酸酰胺、油酸酰胺和聚二甲基硅氧烷。
根据另一实施例,通过掺入较高量的颜料,抗刮擦性得到改善。
本发明的组合物优选地具有低于0.99g/cm3的密度(ISO 1183)和5-150g/10min,优选地10-50g/10min的熔体流动速率值(ISO 1133-230℃,2.16Kg)。
本发明的组合物可以通过机械混合其组分来制备。
本发明的组合物适当地示出了弯曲模量(ISO 178)高于1000MPa,优选地高于1200MPa,更优选地高于1400MPa。本发明的组合物还适当地示出了拉伸模量高于1000MPa,优选地高于1200MPa,更优选地高于1400MPa。
根据本发明的组合物有利地示出了在标准“气味试验”中的改进,在反应器外而不是经由过氧化物减粘裂化获得聚合物组分的高的流动性。
由于还提供低密度值之外的高刚度、高流动性和良好的冲击特性的性能结合,本发明的组合物特别适合用于模制品(例如,汽车工业的成品零件)。
因此,本发明的另一目的是用根据本发明的组合物制成模制品。根据本发明的所述模制品,例如,可以是汽车工业的成品零件(例如,用于汽车的仪表盘、仪表板或其他内部或外部装饰组件)。
根据另一目的,本发明提供了包含有根据本发明的模制品的车辆(例如,汽车或卡车)。
具体实施方式
下面给出实施例来说明本发明而无任何限制性目的。
测量方法
根据下面的方法获得丙烯聚合物和获得的膜的特征化数据:
密度
在没有不同的指定的情况下,根据ISO 1183确定。
熔体流动速率(MFR)
在没有不同的指定的情况下,根据ISO 1133(230℃,2.16Kg)确定。
多分散指数(PI)
聚合物占分子量分布的比例。为了确定PI值,在低模量值(例如,500Pa)处的模量分离通过使用由Rheometrics(美国)销售的型号RMS-800的平行板流变仪在200℃的温度下确定,在从0.01弧度/秒至100弧度/秒增加的振荡频率下操作该平行板流变仪。可以使用下面的等式从模量分离值导出PI:
PI=54.6x(模量分离)-1.76
其中模量分离(MS)被定义为:
MS=(在G′=500Pa下的频率)/(在G″=500Pa下的频率)
其中G′是储能模量并且G″是低模量。
弯曲模量
根据ISO方法178确定。
拉伸模量
根据ISO 527/1+2确定。
夏比冲击强度
根据ISO 179/1eU和ISO 179/1eA确定。
抗刮擦性:
使用了刮擦设备的硬金属尖头(其具有限定的几何形状)以限定的速率和在粗化表面上的接触力来产生划痕网格。
在10N载荷、1000毫米/分钟速率下在Erichsen刮擦设备型号430上根据Volkswagen AG公的PV 3952 2002刮擦方法测量了抗刮擦性。使用色度计在刮擦之前和之后测量了亮度差异(dL)。较小的亮度差异(dL)值指示更好的抗刮擦性能。
二甲苯可溶物(XS)
确定如下:将2.5g聚合物和250ml的二甲苯引入配备有致冷器和磁力搅拌器的玻璃烧瓶中。将温度在30分钟内升高到溶剂的沸点。然后将如此获得的透明溶液在回流和搅拌下再保持30分钟。然后将密闭的烧瓶在25℃的恒温水浴中保持30分钟。在快速滤纸上过滤如此形成的固体。将100ml的滤液注入预先称重的铝容器中,该铝容器在氮气流下在加热板上被加热,以通过蒸发去除溶剂。然后将容器保持在80℃下的真空烘箱中,直到获得恒定重量。然后计算在室温下可溶于二甲苯的聚合物的重量百分比。
硬度
邵氏A根据ISO 868在模压板(厚度4mm)上测量。
根据下面的内部测试方法的纵向(MD)和横向(TD)模具收缩率
24小时后测量板块和薄膜浇口的整个宽度,以确保熔体均匀的流动和方向。在注模机“Demag 160”(其中160代表160吨夹紧力)中,模制195x100x2.5毫米大小的板块。
注塑条件是:
熔体温度=210℃;
注塑成型压强:=80巴
模制温度=30℃;
注塑时间=11秒;
保持压强=50巴;
保持时间=30秒;
冷却时间=20秒
循环时间=76秒;
螺杆转速=80转/分(1/分)。
在模制(模内收缩)24小时后和在80℃退火(总收缩)48小时之后通过卡钳测量板块,收缩率由下式给出:
纵向收缩(MD)=(195-读取值)/195*100
横向收缩(TD)=(100-读取值)/100*100
其中195是在模制后立即测量的板块沿流向的长度(MD)(以毫米计);100是在模制后立即测量的板块横跨流向的长度(TD)(以毫米计);读取值是在相关方向的板块长度。
线性热膨胀系数(CLTE)-ASTM D696。
使用公式计算CLTE(α):α=ΔL/(Lo*ΔT),其中ΔL是样品的长度变化值,Lo是样品原始长度值,并且ΔT是测试期间的温度变化值。
实施例
在实施例中描述的所有组合物是由双螺杆挤出机Krupp Werner&Pfleiderer/1973,ZSK 53(螺杆直径:2×53.36D)以150转/分的螺杆转速和230℃的溶解温度进行生产的。
所有的化合物均由Battenfeld BA 1500/630注塑机在相同工艺条件下注塑模制,所述工艺条件是熔体温度:220℃、模具温度:35℃,注塑压强:1500巴。
实施例1(比较实施例)-组合物
所述组合物由以下成分构成:
14%HECO6,异相丙烯共聚物具有2.2g/10min的MFR(ISO 1133-230℃,2.16Kg);
45%HECO5,异相丙烯共聚物具有11g/10min的MFR(ISO 1133-230℃,2.16Kg);
16%HECO4,异相丙烯共聚物具有11g/10min的MFR(ISO 1133-230℃,2.16Kg);
22%来自IMERYS的滑石SteamicT1CA(水合硅酸镁,d50(沉降图5100)=2.0,层状指数=1.8);
3%预混合料:购自Lyondellbasell的2.1%MP HF501N(薄片)均聚物,其密度是0.9g/cm3、熔体流动速率(MFR)是10g/10min(230℃/2.16Kg)、拉伸模量1550MPa;0.4%植物油酸酰胺(油酸酰胺V);0.2%氧化镁;0.1%Ethanox 330(抗氧剂1330);Songnox1680(M.S.168);0.1%碳黑PFEB(黑色颜料)。
该丙烯聚合物组分和最终组合物的主要性质报道在表1和表2中。
实施例2-组合物
所述组合物由以下成分构成:
20%PPI,丙烯均聚物具有15极高的PI(多分散指数),25g/10min的MFR(ISO 1133-230℃,2.16Kg);1200MPa的弯曲模量;
20%TAFMER,A-1050S乙烯-1-丁烯共聚体弹性材料,(三井化学制品股份有限公司的注册商标),密度:0.864g/cm3,熔体流动速率:190℃测得为1.4g/10min。在2.16千克负载下,1-丁烯单元含量:31.8wt%(按摩尔计18.9%);硬度是57点(邵氏A);
45%HECO1,异相丙烯共聚物具有17.1g/10min的MFR(ISO 1133-230℃,2.16Kg);1020MPa弯曲模量;
12%来自IMERYS的滑石Steamic T1CA(水合硅酸镁,d50(沉降图5100)=2.0,层状指数=1.8);
3%预混合料:2.1%MP HF501N(薄片);0.4%植物油酸酰胺(油酸酰胺V);0.2%氧化镁;0.1%Ethanox 330(抗氧剂1330);Songnox 1680(M.S.168);0.1%碳黑PFEB(黑色颜料)。
丙烯聚合物组分和最终组合物的主要性质报道在表1和表2中。
实施例3(比较实施例)-组合物
所述组合物由以下成分构成:
6%HDPE1,高密度聚乙烯(HDPE)具有8g/10min的MFR(ISO 1133-190℃,2.16Kg);1200MPa弯曲模量;
29%HECO3,异相丙烯共聚物具有18g/10min的MFR(ISO 1133-230℃,2.16Kg);1650MPa弯曲模量;
28%HECO2,异相丙烯共聚物具有72g/10min的MFR是(ISO 1133-230℃,2.16Kg);1140MPa弯曲模量;
10%TAFMER,A-1050S乙烯-1-丁烯共聚物弹性材料,(三井化学制品股份有限公司的注册商标),密度:0.864g/cm3,熔体流动速率:190℃测得为1.4g/10min。在2.16千克负载下,1-丁烯单元含量:31.8wt%(按摩尔计18.9%);硬度是57点(邵氏A);
20%来自IMERYS的滑石Steamic T1CA(水合硅酸镁,d50(沉降图5100)=2.0,层状指数=1.8);
7%预混合料:2%在标准聚丙烯均聚物中的50%聚二甲基硅氧烷母料;2%黑母料40%黑;0.4%抗氧剂B225;0.1%光稳定剂3853PE;0.15%氧化镁;0.1%乙撑双硬脂酰胺(EBS);2.25%颜料和MPHF 501N。
该丙烯聚合物组分和最终组合物的主要性质报道在表1和表2中。
实施例4(比较实施例)-组合物
所述组合物由以下成分构成:
6%HDPE1,高密度聚乙烯(HDPE)具有8g/10min的MFR(ISO 1133-190℃,2.16Kg);1200MPa弯曲模量;
62.5%HECO3,异相丙烯共聚物具有18g/10min的MFR(ISO 1133-230℃,2.16Kg);1650MPa弯曲模量;
13%TAFMER,A-1050S乙烯-1-丁烯共聚物弹性材料,(三井化学制品股份有限公司的注册商标),密度:0.864g/cm3,熔体流动速率:190℃测得为1.4g/10min。在2.16千克负载下,1-丁烯单元含量:31.8wt%(按摩尔计18.9%);硬度是57点(邵氏A);
12%购自IMERYS的滑石Steamic T1CA(水合硅酸镁,d50(沉降图5100)=2.0,层状指数=1.8);
6.5%预混合料:1.5%在PP2%黑母料40%黑中的50%聚二甲基硅氧烷母料;0.4%抗氧剂B225;0.1%光稳定剂3853PE;0.15%氧化镁;0.1%乙撑双硬脂酰胺(EBS);2.25%颜料和MP HF 501N。
实施例5-组合物
所述组合物由以下成分构成:
6%HDPE1,高密度聚乙烯(HDPE)具有8g/10min的MFR(ISO 1133-190℃,2.16Kg);1200MPa弯曲模量;
40.5%HECO1,异相丙烯共聚物具有17.1g/10min的MFR(ISO 1133-230℃,2.16Kg);1020MPa弯曲模量;
27%PP1,丙烯均聚物具有15的极高的PI(多分散指数),25g/10min的MFR(ISO1133-230℃,2.16Kg),2120MPa弯曲模量;
10%TAFMER A-1050S乙烯-1-丁烯共聚物弹性体,(三井化学公司(MitsuiChemicals,Inc.)的商品名),密度:0.864g/cm3,熔体流动速率:1.4g/10min,在2.16kg的荷载下在190℃下测得,1-丁烯的单位含量:31.8wt%(按摩尔计18.9%);硬度是57点(邵氏A);
10%来自IMERYS的滑石LUZENAC HAR T84(水合硅酸镁,d50(沉降图5100)=2.0,层状指数=4.3);
6.5%预混合料:1.5%在PP中的50%聚二甲基硅氧烷母粒;2%炭黑母料,40%碳黑;0.4%抗氧化剂B225;0.1%光稳定剂3853PE;0.15%氧化镁;0.1%EBS;2.25%颜料和MPHF 501N。
该组合物的聚合物组分的主要性质报道在表1中。
表2中报道了该组合物的组分含量和最终性质。
表1
*在橡胶组分中的平均数
表2
表2续
已认为HDPE组分(C)有助于“基质”,而认为TAFMER金属茂共聚物弹性体有助于组合物中的“橡胶”部分。根据数据显示,显然在根据本发明所述的组合物中滑石含量的减少能够在维持冲击力和刚度且不会加剧收缩。
特别地,对比实施例4显示减少滑石对于降低密度有效,但是不可避免地会使刚度(弯曲模量)变差。聚合物组分的含量和类型必须根据本发明有目的地进行选择,以保持减少滑石后所需的性质平衡。
Claims (9)
1.一种密度小于1g/cm3的组合物,包括:
(A)15-60wt%的一种或多种丙烯基组分,所述丙烯基组分选自丙烯均聚物、丙烯共聚物或其组合,此类第一丙烯基的组分具有根据ISO178测得的大于1500MPa的弯曲模量,以及大于10的PI;
(B)20-50wt%的异相丙烯聚合物,其具有根据ISO 1133在230℃、在2.16kg负载下测得的10-20g/10min的熔体流动速率,所述异相丙烯聚合物包括:
(B1)50-90wt%的结晶聚丙烯,其具有室温下在二甲苯中小于5wt%的所述组分(B1)的溶解度,以及根据ISO 1133在230℃、在2.16kg负载下测得的大于50g/10min的熔体流动速率;
(B2)10-50wt%的乙烯与作为共聚单体的至少一种C3-C10α-烯烃的共聚物,该共聚物含有40-60wt%的乙烯,其在室温下在二甲苯中的溶解度大于70wt%;
(D)5-25wt%的乙烯基塑性体或弹性体,其具有根据ASTM D-2240测得的等于或小于90点的邵氏A硬度,小于0.890g/cm3的密度;
(E)1-15wt%的滑石;
(C)0-10wt%的高密度聚乙烯(HDPE);并且
其中所述组合物具有1)高于1400MPa的弯曲模量;2)高于1000MPa的拉伸模量,并且所述组合物中组分的百分含量总和等于100%。
2.根据权利要求1所述的组合物,其中所述组合物包含20-30wt%的组分(A)。
3.根据权利要求1或2所述的组合物,其中所述组分(A)具有根据ISO 178测得的大于2000MPa的弯曲模量和大于13的PI。
4.根据权利要求1或2所述的组合物,其中所述组分(A)具有根据ISO 1133在230℃、在2.16kg负载下测得的10-150g/10min的MFR值。
5.根据权利要求1或2所述的组合物,其中所述组分(B1)具有根据ISO 1133在230℃、在2.16kg负载下测得的大于70g/10min的熔体流动速率MFR值。
6.根据权利要求1或2所述的组合物,其中所述组分(E)是具有等于或高于2.8的层状指数的高纵横比滑石。
7.一种由根据前述任一项权利要求所述的组合物制备成的模制品。
8.根据权利要求7所述的模制品,其作为成品零件用在汽车工业中。
9.一种车辆,其包括根据权利要求8所述的模制品。
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SG11201810453PA (en) * | 2016-05-31 | 2018-12-28 | Dow Global Technologies Llc | Thermoplastic polyolefin blends including ethylene rich polymers |
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TW201811976A (zh) | 2016-08-08 | 2018-04-01 | 美商堤康那責任有限公司 | 用於散熱器之導熱聚合物組合物 |
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WO2018114977A1 (en) * | 2016-12-23 | 2018-06-28 | Sabic Global Technologies B.V. | Automotive part |
US11807745B2 (en) | 2016-12-23 | 2023-11-07 | Sabic Global Technologies B.V. | Interior automotive part |
EP3559110B1 (en) | 2016-12-23 | 2022-09-07 | SABIC Global Technologies B.V. | Exterior or semi-exterior automotive part |
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EP3710532B1 (en) * | 2017-11-13 | 2023-05-24 | Basell Poliolefine Italia S.r.l. | Compositions obtained from recycled polyolefins |
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