CN111278908A - 由回收聚烯烃获得的组合物 - Google Patents

由回收聚烯烃获得的组合物 Download PDF

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CN111278908A
CN111278908A CN201880069156.1A CN201880069156A CN111278908A CN 111278908 A CN111278908 A CN 111278908A CN 201880069156 A CN201880069156 A CN 201880069156A CN 111278908 A CN111278908 A CN 111278908A
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polyolefin composition
component
composition according
ethylene
propylene
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R·迪帕洛
C·卡瓦列里
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Basell Poliolefine Italia SRL
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Abstract

一种聚烯烃组合物，其包括：T1)70wt％至95wt％的聚烯烃组分，其包括：a1)30wt％至70wt％的丙烯基聚合物；和a2)30wt％至70wt％的乙烯基聚合物；T2)5wt％至30wt％的多相丙烯乙烯共聚物。

Description

由回收聚烯烃获得的组合物
技术领域
本发明涉及由含有包括丙烯乙烯共聚物作为增容剂的组合物的回收聚烯烃获得的组合物。
背景技术
聚烯烃，特别是聚乙烯和聚丙烯，在许多应用中消耗量越来越大，包括食品和其他商品的包装、纤维、汽车零部件和各种各样的制成品。然而，上述聚烯烃的大量使用引起了人们对第一次使用后产生的废物对环境影响的关注。
实际上，目前大量的塑料废弃物主要来源于城市塑料废弃物的差别化回收，主要包括软包装(流延膜、吹塑膜和BOPP薄膜)、硬包装、吹塑瓶和注塑容器。通过与其他聚合物如PVC、PET或PS分离的步骤，获得两种主要的聚烯烃级分，即聚乙烯(特别是LDPE，LADE)和聚丙烯(均聚物、无规共聚物、多相共聚物)。
聚烯烃回收利用的关键问题之一是聚丙烯(PP)和聚乙烯(PE)难以定量分离，特别是在处理用后废弃物(PCW)的物流时。已经发现，来自PCW来源的商业回收物通常含有PP和PE的混合物，次要组分含量可达<50wt％。
这种回收的PP/PE共混物通常具有劣化的机械和光学性能，气味和味道较差，并且它们通常在主聚合物相之间具有较差的相容性，导致冲击强度和抗热挠曲性有限。由于PCW中PE组分的粘度通常较高，即使在高达65％的PP浓度下，这种较差的性能也部分地由具有形成连续相的较低刚度和熔点的PE引起。
这些缺点通常排除了高质量部件的应用，并且它仅允许在低成本和非苛刻的应用中使用。
为了提高PP与PE的相容性，进行了一些研究。根据Wei Zhu等人；″应用聚合物科学杂志(Journal of Applied Polymer Science)”第58卷，p.515-521(1995)，将乙烯-丙烯共聚物作为增容剂添加到聚丙烯和聚乙烯的共混物中可以在一定程度上补救高不相容性的情况，并且乙烯-丙烯橡胶(EPR)或乙烯-丙烯-二烯橡胶(EPDM)可以显著改善共混物的韧性，但以降低模量和拉伸强度为代价。
WO2013075241 A1还公开了使用乙烯-丙烯-二烯橡胶(EPDM)或无规乙烯-丙烯共聚物(EP-RACO)作为回收塑料共混物的增容剂的方法。
现已发现，包括丙烯基聚合物和线性低密度聚乙烯(LLDPE)的组合物可用作该混合物的增容剂，从而允许更好的性能，特别是用于生产膜。
发明内容
本发明涉及聚烯烃组合物，其包括：
T1)70wt％至95wt％的聚烯烃组分，其包括：
a1)30wt％至70wt％的丙烯含量高于60wt％的丙烯基聚合物；
a2)30wt％至70wt％的乙烯含量高于70的乙烯基聚合物；
a1)和a2)之和，即a1)和a2)的总重量为100；
T2)5wt％至30wt％的多相丙烯乙烯共聚物，其具有：
i)6.0wt％至16.0wt％的乙烯衍生单元含量；
ii)15wt％至45wt％的252℃下二甲苯可溶物级分(XS)；
iii)4.0-9.0dl/g的25℃下二甲苯可溶物级分的特性粘度(η)；
iv)根据ISO 1133在230℃下以2.16kg的负荷测量的0.3-50.0g/10min的熔体流动速率；
T1)+T2)的量之和，即T1)和T2)的总重量为100；
具体实施方式
本发明涉及聚烯烃组合物，其包括：
T1)70wt％至95wt％，优选75wt％至90wt％；更优选77wt％至85wt％的聚烯烃组分，其包括：
a1)30wt％至70wt％，优选40wt％至60wt％，更优选45wt％至55wt％丙烯含量高于60wt％；优选高于70wt％；更优选高于80wt％，甚至更优选高于90wt％的丙烯基聚合物
a2)30wt％至70wt％，优选40wt％至60wt％，更优选45wt％至55wt％的具有高于70wt％，优选高于75wt％；更优选高于80wt％，甚至更优选高于90wt％的乙烯含量的乙烯基聚合物；
a1)和a2)之和，即a1)和a2)的总重量为100；
T2)5wt％至30wt％，优选10wt％至25wt％；更优选15wt％至23wt％的多相丙烯乙烯共聚物，其具有：
i)6.0wt％至16.0wt％，优选为8.0wt％至14.0wt％；更优选为9.0wt％至12.0wt％的乙烯衍生单元含量；
ii)15wt％至45wt％；优选20wt％至40wt％；更优选30wt％至35wt％的252℃下二甲苯可溶物级分(XS)；
iii)4.0-9.0dl/g；优选5.0-8.3dl/g；更优选5.6-7.9dl/g的25℃下二甲苯可溶物级分的特性粘度(η)；
iv)根据ISO 1133在230℃下以2.16kg的负荷测量的0.3-50.0g/10min；优选0.4-20.0g/10min；更优选0.5-4.0g/10min的熔体流动速率。
T1)和T2)的量之和，即T1)和T2)的总重量为100。
多相丙烯乙烯共聚物是包括基质和橡胶相的聚合物，基质包括全同立构丙烯均聚物，橡胶相分散在作为丙烯乙烯共聚物的基质中。
聚烯烃组合物可有利地用于生产膜，包括流延、吹塑和双取向膜单层或多层，其中膜中的凝胶数减少。
组分T1)优选为回收的聚丙烯共混物和回收的聚乙烯共混物的混合物。
更优选地，组分a1)是包括0wt％至5wt％共聚单体的丙烯均聚物，该共聚单体是烯烃衍生的单元，优选具有2至10个碳原子的α烯烃衍生的单元，例如乙烯、1-丁烯、1-己烯和1-辛烯衍生的单元；优选乙烯，更优选使用丙烯均聚物。
更优选地，组分a2)是包括0wt％至20wt％共聚单体的乙烯均聚物或共聚物，该共聚单体是烯烃衍生的单元，优选具有3至10个碳原子的α烯烃衍生的单元，例如丙烯、1--丁烯、1--己烯和1--辛烯衍生的单元；优选1-丁烯和1-己烯。
组分T2)是商业丙烯乙烯共聚物，例如由LyondellBasell销售的Hifax X1956A级。
给出以下实施例是为了说明而非限制本发明。
实施例
表征
25℃下二甲苯可溶物(XS)级分
二甲苯中的溶解度：测定如下：
将2.5g聚合物和250ml二甲苯引入装配有冰箱和磁力搅拌器的玻璃烧瓶中。在30分钟内将温度升高至溶剂的沸点。然后将所得澄清溶液保持回流并搅拌30分钟。然后将封闭的烧瓶在冰水浴中保持30分钟，然后在25℃的恒温水浴中保持30分钟。所得固体在快速滤纸上过滤。将100ml过滤的液体倒入预先称重的铝容器中，该铝容器在氮气流下在加热板上加热以通过蒸发除去溶剂。然后在真空下将容器保持在80℃的烘箱上，直到获得恒定重量。然后计算室温下可溶于二甲苯的聚合物的重量百分比。
二甲苯可溶物级分的含量表示为原始2.5克的百分比，然后通过差值(与100％互补)表示二甲苯不溶百分比(％)。
熔体流动速率(MFR)
根据ISO 1133在230℃下以2.16kg的负荷测量。
特性粘度(IV)
将样品在135℃溶解在四氢化萘中，然后倒入毛细管粘度计中。粘度计管(乌式)由圆柱形玻璃夹套包围；这种设置允许用循环恒温液体进行温度控制。弯液面的下行通道由光电装置计时。
上部灯前的弯液面通道启动具有石英晶体振荡器的计数器。弯液面在计数器通过下部灯时使计数器停止，并记录流出时间：假设已知在相同的实验条件(相同的粘度计和相同的温度)下的纯溶剂的流动时间，通过Huggins方程(Huggins，M.L.，《美国化学会志》(J.Am.Chem.Soc.)，1942，64，2716)将其转换成特性粘度值。使用一种单一聚合物溶液测定[η]。
共聚物中乙烯的含量
在装有低温探针的Bruker AV-600光谱仪上获得13C NMR光谱，在120℃下以傅里叶变换模式160.91MHz进行操作。
Sββ碳(根据″Monomer Sequence Distribution in Ethylene-Propylene RubberMeasured by 13C NMR.3.Use of Reaction Probability Mode(通过13C NMR测量的乙烯-丙烯橡胶中的单体序列分布.3.反应概率模式的使用)″CJ Carman，RA Harrington和CEWilkes，Macromolecules(大分子)，10，536(1977)的命名法)的峰在29.9ppm处用作内参照。在120℃和8％wt/v浓度下将样品溶解在1，1，2，2-四氯乙烷-d2中。用90°脉冲获得每个光谱，脉冲和复合脉冲解耦(CPD)之间15秒的延迟可除去任何1H-13C偶联。使用9000Hz的光谱窗将512个瞬态存储在32K数据点中。
光谱的分配，三价基分布的评价和组成是根据Kakugo(″Carbon-13NMRdetermination of monomer sequence distribution in ethylene-propylenecopolymers prepared with δ-titanium trichloride-diethylaluminum chloride(碳-13NMR测定由δ-三氯化钛-二乙基氯化铝制备的乙烯-丙烯共聚物中的单体序列分布)″M.Kakugo，Y Naito，K.Mizunuma和T.Miyatake，Macromolecules(大分子)，15，1150(1982))使用以下等式进行的：
PPP＝100Tββ/S PPE＝100Tβδ/S EPE＝100Tδδ/S
PEP＝100Sββ/S PEE＝100Sβδ/S EEE＝100(0.25Sγδ+0.5Sδδ)/S
S＝Tββ+Tβδ+Tδδ+Sββ+Sβδ+0.25Sγδ+0.5Sδδ
使用以下等式测定乙烯含量的摩尔百分比：
E％mol＝100*[PEP+PEE+EEE].此外，使用以下等式评价乙烯含量的重量百分比：
Figure BDA0002463520680000061
其中P％mol是丙烯含量的摩尔百分比，而MWE和MWP分别是乙烯和丙烯的分子量。
竞聚率r1r2的乘积根据Carman(C.J.Carman，R.A.Harrington and C.E.Wilkes，Macromolecules(大分子)，10，536(1977)计算为：
Figure BDA0002463520680000062
丙烯序列的立构规整度由PPP mmTββ(28.90-29.65ppm)和整个Tββ(29.80-28.37ppm)的比率计算为mm含量
T1组分的生产
为了模拟废弃回收得聚烯烃组合物，已经获得了50wt％的霍斯塔纶(hostalen)GF9055F(由LyondellBasell销售的商业高密度聚乙烯)和50wt％的
LyondellBasell出售的聚丙烯均聚物Moplen(莫普纶等规聚丙烯纤维)HP561R的共混物。
T1组分已经与各种丙烯基共聚物共混，并且用所得组合物获得流延膜，膜的组成和凝胶数列于表1中
表1
Figure BDA0002463520680000071
Adflex X500F是LyondellBasell销售的多相组合物，通常用于共挤出流延膜和注塑应用。Adflex X500F具有约57wt％的乙烯含量；25wt％的25℃下二甲苯可溶物级分。25℃下二甲苯可溶物级分的特性粘度为1.34dl/g，MFR为约7g/10min。
Hifax X 1956A是由LyondellBasell销售的多相TPO(热塑性聚烯烃)聚丙烯级。Hifax X 1956具有11.0wt％的乙烯含量；29wt％的25℃下二甲苯可溶物级分。25℃下二甲苯可溶物级分的特性粘度为6.8dl/g且MFR为1.7g/10min。
凝胶计数试验在具有25mm单螺杆的流延膜Collin挤出生产线直径上进行，具有以下特征：
单螺杆L/D 25
温度曲线
圆筒200(靠近料斗)→230℃(在挤出机的末端，在进入模具之前)
模具240℃
模具宽度150mm
冷却辊30℃
膜速度3.0m/min
膜厚50微米
检查面积1m2
4cm宽带上的OCS FS5凝胶计数单元
实施例2和对比实施例1和3的流延膜的断裂伸长率已经根据表2中的ASTM D 882在纵向(MD)和横向(TD)上测量。实施例2在两个方向上的断裂伸长率值相当的事实是该共混物已经被增容的指标。
表2
Figure BDA0002463520680000081
Figure BDA0002463520680000091

Claims (15)

1.一种聚烯烃组合物，其包括：
T1)70wt％至95wt％的聚烯烃组分，其包括：
a1)30wt％至70wt％的丙烯含量高于60wt％的丙烯基聚合物；和
a2)30wt％至70wt％的乙烯含量高于70的乙烯基聚合物；
a1)和a2)之和，即a1)和a2)的总重量为100；
T2)5wt％至30wt％的多相丙烯乙烯共聚物，其具有：
i)6.0wt％至16.0wt％的乙烯衍生单元含量；
ii)15wt％至45wt％的252℃下二甲苯可溶物级分(XS)；
iii)4.0-9.0dl/g的25℃下二甲苯可溶物级分的特性粘度(η)；
iv)根据ISO 1133在230℃下以2.16kg的负荷测量的0.3-50.0g/10min的熔体流动速率；
T1)和T2)的量之和，即T1)和T2)的总重量为100；
2.根据权利要求1所述的聚烯烃组合物，其中组分T2包括8.0wt％至14.0wt％的乙烯衍生单元。
3.根据权利要求1或2所述的聚烯烃组合物，其中组分T2包括9.0wt％至12.0wt％的乙烯衍生单元。
4.根据权利要求1至3中任一项所述的聚烯烃组合物，其中组分T2具有0.4-20.0g/10min的熔体流动速率。
5.根据权利要求1至4中任一项所述的聚烯烃组合物，其中组分T2具有0.5-4.0g/1Omin的熔体流动速率。
6.根据权利要求1至5中任一项所述的聚烯烃组合物，其中组分T2具有5.0-8.3dl/g的25℃下二甲苯可溶物级分的特性粘度(η)。
7.根据权利要求1至6中任一项所述的聚烯烃组合物，其中组分T2具有5.6-7.9dl/g的25℃下二甲苯可溶物级分的特性粘度(η)。
8.根据权利要求1至7中任一项所述的聚烯烃组合物，其中组分T2具有20wt％至40wt％的252℃下二甲苯可溶物级分(XS)。
9.根据权利要求1至8中任一项所述的聚烯烃组合物，其中所述聚烯烃组合物具有0.5-25g/10m的熔体流动速率(230℃/2.16kg)；
10.根据权利要求1至9中任一项所述的聚烯烃组合物，其中组分a1)为45wt％至55wt％且组分a2)为40wt％至60wt％。
11.根据权利要求1至10中任一项所述的聚烯烃组合物，其中组分T1)是回收的聚丙烯和聚乙烯共混物的混合物。
12.根据权利要求1至11中任一项所述的聚烯烃组合物，其中组分a1)是丙烯均聚物，其包括0至5wt％的为烯烃衍生单元的共聚单体。
13.根据权利要求1至12中任一项所述的聚烯烃组合物，其中a2)是乙烯均聚物或共聚物，其包括0至20wt％的为烯烃衍生单元的共聚单体的。
14.一种膜，其包括根据权利要求1至13所述的聚烯烃组合物。
15.根据权利要求114所述的膜，其为流延、吹塑或双向取向膜，单层或多层。
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