CN115505185B - 一种聚乙烯功能母粒及其制备方法、包含该母粒的树脂组合物 - Google Patents
一种聚乙烯功能母粒及其制备方法、包含该母粒的树脂组合物 Download PDFInfo
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- CN115505185B CN115505185B CN202110634523.1A CN202110634523A CN115505185B CN 115505185 B CN115505185 B CN 115505185B CN 202110634523 A CN202110634523 A CN 202110634523A CN 115505185 B CN115505185 B CN 115505185B
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Abstract
本发明涉及一种聚乙烯功能母粒,该聚乙烯功能母粒以聚乙烯功能母粒为100质量份计,由以下组分制备而成:(A)聚乙烯40~60质量份;(B)氯化聚乙烯30~50质量份;(C)包含式(I)所示结构单元的聚合物1~15质量份;其中,R1为含有8~32个碳原子的烷基;R2为C6H5或COOR,R为烷基;R3为H或CH3;3≤n≤100;所述组分(A)聚乙烯为乙烯均聚物,在温度190℃、负荷2.16Kg下的熔体流动速率MFR为20~300g/10分钟,密度≥0.955g/cm3。本发明还涉及一种上述聚乙烯功能母粒的制备方法以及一种树脂组合物。含有该聚乙烯功能母粒的树脂组合物的耐热性能有明显提高。
Description
技术领域
本发明属于聚烯烃树脂领域,特别涉及一种聚乙烯功能母粒及其制备方法、包含该聚乙烯功能母粒的树脂组合物。
背景技术
聚乙烯(PE)是经乙烯聚合制得的一种热塑性树脂。聚乙烯树脂的化学稳定性好,能耐大多数酸碱的侵蚀,而且电绝缘性优良,用途十分广泛,可用于制作薄膜、包装材料、容器、管道、单丝、电线电缆、日用品等,也可用于电视、雷达等所需的高频绝缘材料。但是聚乙烯的耐热性不高,热变形温度低,限制了聚乙烯在某些耐温领域的应用。
为提高聚乙烯的耐热性能,可以直接对聚乙烯进行化学接枝改性。文献“耐热聚乙烯薄膜的研究”(华侨大学学报(自然科学版),1994(04):397-400)介绍了低密度聚乙烯接枝甲基丙烯酸甲酯制成的薄膜有一定耐热性,接枝度为17.4%~23.0%的薄膜耐热温度可提高至140℃。文献“聚乙烯薄膜接枝甲基丙烯酸的研究”(塑料工业,1992(04):26-28)介绍了α-甲基丙烯酸在LDPE薄膜上进行的接枝改性。当接枝率为30~50%时接枝薄膜的耐热性最好,其软化点为130~175℃。
上述通过有机物改性的方法可以提高聚乙烯的耐热性,但这种方法对于聚乙烯颗粒原料不具有普适性,且需要较高的接枝率才能达到目的。接枝效率受反应条件影响较大,不利于工业化生产应用。
另外一类提高聚乙烯耐热性能最常用的方法是在聚乙烯树脂中添加耐热的无机物进行改性。CN201810547451.5通过热塑性聚氨酯弹性体、改性高岭土、改性纳米二氧化硅、碳纤维共同作用改善聚乙烯耐热性。CN201510283310.3通过钛酸钾晶须以及氟树脂、长碳链聚酰胺两种特定含量的有机材料混合作用于超高分子量聚乙烯材料,提高产品的耐热性。
上述方法需要添加较大量的无机物以提高聚乙烯的耐热性能,多用于有一定厚度的产品,不适用于薄膜等领域。
CN201510436899.6公开了包含聚丙烯酸酯、纳米碳酸钙等的耐热高强度PE管材。CN201510110792.2公开了包含以下组分的韧性优高耐候性改性塑料:线性低密度聚乙烯100、聚醚0.3-0.6、聚丙烯酸酯2-4、纳米氧化锡锑3.4-6.7、纳米钛白粉1.2-2.1、有机锡0.2-0.4、氧化硼0.3-0.5、乙氧基月桂酷胺0.4-0.6、硬脂酸钙2-3、沸石粉1-3、苯基三甲氧基硅烷1-2、无水乙醇适量;所述材料的制作方法包括以下步骤:(1)将纳米氧化锡锑、纳米钛白粉于580-770℃下煅烧处理30-50分钟,冷却放入三口烧瓶内,加入无水乙醇、苯基三甲氧基硅烷搅拌均匀,加热回流4-5h,离心分离,用无水乙醇洗涤2~3次,80℃下真空干燥;(2)将上述产品中加入沸石粉、硬脂酸钙搅拌混合均匀,制得混合粉体;(3)将线性低密度聚乙烯加入到高速混合分散机中,加入上述混合粉体、聚醚及其它剩余成分混合分散15-20分钟,取出倒入双螺杆挤出机中,按操作规程挤出,经造粒机造粒,出料。这些现有技术中聚乙烯耐热性的提高有限;材料的制备基本采用聚乙烯组分和其他组分掺混,各种无机填料作为耐热组分,聚丙烯酸酯作为抗冲改性剂提高了组合物或产品的韧性。
CN201710026350.9公开了提高聚乙烯耐热性的功能母粒,通过聚双马来酰亚胺树脂、碳化硅纤维、纳米级二氧化硅粉、纳米级萤石粉等共同作用提高聚乙烯耐热性。此方法同样需要添加无机物,并且需要将聚双马来酰亚胺树脂与聚乙烯进行共混交联,交联后聚乙烯就失去了可以热塑性加工以及循环使用的优势。
CN201810505938.7公开了包括主树脂、辅助树脂、离聚物树脂、抗氧剂的高熔点耐热型透明聚乙烯薄膜。其中离聚物树脂为自由基聚合的乙烯、丙烯等聚α烯烃与丙烯酸酯类单体共聚而成,生产难度较大。
由上可知,现有技术中仍缺少简单易行能提高聚乙烯耐热性能的方法。
发明内容
基于以上所述,本发明的目的是提供一种聚乙烯功能母粒及其制备方法、包含该聚乙烯功能母粒的树脂组合物,含有该聚乙烯功能母粒的树脂组合物的耐热性能有明显提高。
为此,本发明提供一种聚乙烯功能母粒,以聚乙烯功能母粒为100质量份计,由以下组分制备而成:
(A)聚乙烯40~60质量份;
(B)氯化聚乙烯30~50质量份;
(C)包含式(I)所示结构单元的聚合物1~15质量份;
其中,R1为含有8~32个碳原子的烷基;R2为C6H5或COOR,R为烷基;R3为H或CH3;3≤n≤100;式(I)中省略了聚合物中除结构单元外还有的端基等。
其中,所述组分(A)聚乙烯为乙烯均聚物,在温度190℃、负荷2.16Kg下的熔体流动速率MFR为20~300g/10分钟,密度≥0.955g/cm3。
具体的,在本发明所公开的功能母粒中,由于聚乙烯(A)、氯化聚乙烯(B)和聚合物(C)三组分共同存在,使得组分(A)能够形成完善的晶区,组分(C)中的极性基团R2与组分(B)氯化聚乙烯的氯原子由于极性协同相互作用形成以氯化聚乙烯为内层,极性基团R2为中间层,长链烷基R1为外层的复合结构。长链烷基R1分散于聚乙烯中提高了组分(B)、(C)和聚乙烯的相容性。最终形成聚乙烯晶区被组分(B)、(C)组装聚集体贯穿的双连续相结构,组分(B)、(C)组装的聚集体形成了晶区之间的联结,在受热时由于晶区和晶区之间有较强的分子链连接,从而不易断裂,提高了聚乙烯功能母粒的耐热性能。
具体的,所述组分(C)聚合物可以由卤代烃直接引发单体聚合反应得到,或由可引发此类单体聚合的基团对长链脂肪醇进行化学修饰后引发单体聚合反应得到。
现有技术中含有可引发此类单体聚合的基团的化合物都可用于本发明中对长链脂肪醇的羟基进行化学修饰。例如,长链脂肪醇的羟基可以用卤化试剂(如2-溴异丁酰溴)修饰,直接引发单体进行原子转移自由基聚合或单电子转移自由基聚合等得到。文献Macromolecules 2005,38,5425.、J.Polym.Sci.,PartA:Polym.Chem.2004,42,496.中公开了将低分子量聚乙烯的羟基修饰后引发丙烯酸酯类或苯乙烯单体进行原子转移自由基聚合的方法。例如,长链脂肪醇的羟基可以用硫酯基团(如二硫代苯甲酸4-氰基戊酸、α-羧基二硫代苯甲酸丙酯、4-氰基戊酸二硫代苯甲酸等)修饰,引发单体进行可逆加成断裂转移自由基聚合。
具体的,所述组分(C)聚合物可以采用现有的各种聚合技术制备,如有机卤化物在过渡金属卤化物/联吡啶体系下引发单体进行原子转移自由基聚合;或使用Cu0/配体作催化剂,在水或强极性溶剂体系中,采用有机卤化物(RX)引发单体在室温或更低温度下进行单电子转移自由基聚合;或使用含有长脂肪链的RAFT试剂(如2-氰基-2-丙基十二烷基三硫代碳酸酯)引发单体进行可逆加成断裂转移自由基聚合。长链脂肪醇的羟基也可以用硫酯基团(二硫代苯甲酸4-氰基戊酸、α-羧基二硫代苯甲酸丙酯、4-氰基戊酸二硫代苯甲酸)修饰,引发单体进行可逆加成断裂转移自由基聚合。有机卤化物可直接使用卤代烃,如1-溴辛烷、1-氯癸烷、氯代十四烷、溴代十四烷、溴代十六烷、溴代十八烷等,也可由长链脂肪醇的羟基与卤化试剂(如2-溴异丁酰溴)反应生成。
其中所列举的卤化试剂(如2-溴异丁酰溴)、硫酯(二硫代苯甲酸4-氰基戊酸、α-羧基二硫代苯甲酸丙酯、4-氰基戊酸二硫代苯甲酸)仅用于阐述本发明的技术方案。相应的,长链脂肪醇化学修饰后作为引发剂可采用现有技术中的各种聚合方法引发上述单体进行聚合反应得到聚合物(C),所列举的原子转移自由基聚合、单电子转移自由基聚合、可逆加成断裂转移自由基聚合仅用于阐述本发明的技术方案。
本发明所述的聚乙烯功能母粒,其中优选的是,所述组分(A)用量为43~55质量份。
本发明所述的聚乙烯功能母粒,其中优选的是,所述R1选自正辛烷基、正癸烷基、正十二烷基、十四烷基、十六烷基、十八烷基、二十烷基、二十二烷基、二十四烷基、二十六烷基、二十八烷基、三十烷基、三十二烷基中一种。
本发明所述的聚乙烯功能母粒,其中优选的是,所述5≤n≤50。
本发明所述的聚乙烯功能母粒,其中优选的是,所述组分(C)聚合物包含结构单元:-(CH2)14-b-(St)80-、-(CH2)20-b-(nBA)60-、-(CH2)30-b-(MMA)30-或-(CH2)24-b-(tBA)40-,其中,St为苯乙烯,nBA为丙烯酸正丁酯,MMA为甲基丙烯酸甲酯,tBA为丙烯酸叔丁酯。
本发明所述的聚乙烯功能母粒,其中优选的是,所述氯化聚乙烯中氯元素的含量为氯化聚乙烯总质量的20wt%~30wt%。
具体的,所述氯化聚乙烯通过市售或制备获得,为本领域的常规的技术手段。所述氯化聚乙烯得制备方法例如但不限于:由高密度聚乙烯(HDPE)通过氯化反应制备。所述高密度聚乙烯(HDPE)为乙烯与α-烯烃的共聚物,α-烯烃可以是丙烯、丁烯-1、己烯-1中的任一种。高密度聚乙烯(HDPE)满足以下特性:密度为0.935~0.952g/cm3,优选为0.945~0.950g/cm3;熔体流动速率为0.40~0.70g/10min(5.0kg);分子量分布宽度(MW/MN)为10以下,优选为6以下;平均粒径为200~300μm。
本发明所述的聚乙烯功能母粒,其中优选的是,所述氯化聚乙烯中氯元素的含量为氯化聚乙烯总质量的21wt%~25wt%。
本发明所述的聚乙烯功能母粒,其中优选的是,所述组分(A)聚乙烯的密度≥0.958g/cm3。
为此,本发明还提供一种上述的聚乙烯功能母粒的制备方法,将组分(A)聚乙烯、组分(B)氯化聚乙烯和组分(C)聚合物在160℃-290℃下挤出造粒后得到该聚乙烯功能母粒。
为此,本发明还提供一种树脂组合物,由以下组分制备而成:
(N)聚乙烯;
(M)权利要求1-5任一项所述的聚乙烯功能母粒,
其中,以组分(N)聚乙烯的质量为100%计,组分(M)聚乙烯功能母粒的含量为5wt%~20wt%;组分(N)聚乙烯选自HDPE(高密度聚乙烯)、LLDPE(线性低密度聚乙烯)、LDPE(低密度聚乙烯)中的至少一种。
为此,本发明还提供一种树脂组合物的制备方法,将上述功能母粒(M)与聚乙烯(N)掺混得到。
本发明的有益效果如下:
本发明公开的聚乙烯功能母粒中,由于聚乙烯(A)、氯化聚乙烯(B)和聚合物(C)三组分共同存在,使得组分(A)能够形成完善的晶区,组分(C)中的极性基团R2与组分(B)氯化聚乙烯的氯原子由于极性协同相互作用形成以氯化聚乙烯为内层,极性基团R2为中间层,长链烷基R1为外层的复合结构。长链烷基R1分散于聚乙烯中提高了组分(B)、(C)和聚乙烯的相容性。最终形成聚乙烯晶区被组分(B)、(C)组装聚集体贯穿的双连续相结构,组分(B)、(C)组装的聚集体形成了晶区之间的联结,在受热时由于晶区和晶区之间有较强的分子链连接,从而不易断裂,提高了聚乙烯功能母粒的耐热性能。
本发明所公开的树脂组合物,由于功能母粒通过三种组分的协同作用起到提升树脂组合物耐热性能的作用,因此采取先制备功能母粒,再与聚乙烯树脂掺混的方法相比直接在聚乙烯树脂中加入各组分具有分散效果更好使树脂组合物性能更加均匀的优点。
与现有技术相比,本发明不需要加入大量的无机物,得到的功能母粒添加到聚乙烯树脂中可有效提升聚乙烯树脂的耐热性,而且添加后的聚乙烯树脂性能均匀稳定。
具体实施方式
以下对本发明的实施例作详细说明:本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和过程,但本发明的保护范围不限于下述的实施例,下列实施例中未注明具体条件的实验方法,通常按照常规条件。
测试方法:
拉伸屈服应力和断裂伸长率测试标准:GB/T 1040.3-2006;
维卡软化温度测试标准:GB/T 1633-2000,试验条件为A50法(负荷10N,升温速率50℃/±5℃/h)。
原料来源:
聚乙烯(A)的制备:在淤浆或气相低压乙烯聚合装置上,使用齐格勒催化剂、菲利普催化剂、茂金属催化剂等各种现有催化剂,以乙烯为聚合单体,以氢气为分子量调节剂,将乙烯聚合得到聚乙烯(A)。例如,在年产10万吨的乙烯聚合装置上,采用淤浆法并联聚合工艺(两个反应釜采用相同聚合条件),使用高活性齐格勒-纳塔型催化剂(三氯化钛和烷基铝),加入乙烯(8000~9000kg/h),用氢气调节熔体流动速率大小,在温度为75~80℃,压力为0.15~0.25MPa,平均停留时间为50~200分钟条件下进行聚合反应得到聚乙烯(A)。
氯化聚乙烯(B)的制备:制备氯含量(质量分数)在20%~30%的氯化聚乙烯(B),可以采用现有的悬浮氯化法、固相氯化法等。例如,按重量配比,在100份水中依次加入分散剂0.05~0.25份、悬浮稳定剂0.002~0.005份、乳化剂0.01~0.05份,在搅拌条件下加入高密度聚乙烯树脂粉末5~5.5份,充分搅拌后,通过夹套热水加热到35-45℃,再向升温后的水中加入引发剂0.025~0.045份,在密封条件下继续加热到50~60℃后,向二次升温后的水中通入氯气20~40重量份,在温度80~130℃、压力0.1~0.3MPa条件下反应1~3小时。通氯反应完成后,降温到50~60℃,得到氯化的聚乙烯母液,经过滤分离、水洗、中和、离心、干燥,制得含氯量在20~30%的氯化聚乙烯(B)。
使用的分散剂为水溶性的表面活性剂和聚合物。适用的分散剂包括十二烷基苯磺酸钠、硬脂酸钠和硬脂酸钾、聚乙烯醇、聚乙烯吡咯烷、聚甲基丙烯酸钠、聚丙烯酸、聚甲基丙烯酸、聚丙烯酸钠、聚甲基丙烯酸钠、马来酸酐-苯乙烯共聚物等。悬浮稳定剂为环氧乙烷环氧丙烷共聚物,如Pluronic F108、F68、F127、P123等。使用的乳化剂为OP类、吐温类、平平加类及植物油-聚氧乙烯醚类乳化剂。如OP-10、吐温60、平平加0-20、蓖麻油-聚氧乙烯醚等。使用的过氧化物引发剂为过氧化二苯甲酰(BPO),过氧化二异丙苯(DCP)中的一种或两种。
聚乙烯氯含量(质量分数)按标准“GB/T 7139-2002塑料氯乙烯均聚物和共聚物氯含量的测定”中的B法测定。
实施例1
功能母粒由以下组分在250℃下挤出造粒制得:熔体流动速率(MFR)为30g/10分钟,密度为0.958g/cm3的聚乙烯50质量份,含氯量25wt%的氯化聚乙烯40质量份,辛烷基聚苯乙烯10质量份。
辛烷基聚苯乙烯的制备:在100mL精制的无水二氯甲烷中加入5mL正辛醇,在冰水浴下逐滴加入10mL 2-溴异丁酰溴,室温反应24小时后过滤除去不溶物,滤液蒸干溶剂,残余物用二氯甲烷溶解,然后依次用饱和碳酸氢钠水溶液、饱和食盐水洗涤,用无水硫酸钠干燥。继续用石油醚/乙酸乙酯(3/1,v/v)过硅胶柱纯化粗产物,得无色油状物,即为2-溴异丁酸辛酯。在安瓿瓶中依次加入2-溴异丁酸辛酯、CuBr、bpy(联吡啶)和苯乙烯,通过三次冷冻-抽气-解冻循环过程除氧,随后密封置于90℃油浴中反应。反应进行12小时后取出安瓿瓶,并将其投入液氮中,终止反应。产物用四氢呋喃溶解稀释后,通过中性氧化铝柱子除去金属催化剂。所得滤液浓缩后在甲醇中沉淀,重复操作两次四氢呋喃溶解/甲醇沉淀后,所得产物在50℃下真空干燥得到辛烷基聚苯乙烯。
实施例2
功能母粒由以下组分在270℃下挤出造粒制得:熔体流动速率MFR为80g/10分钟、密度为0.960g/cm3的聚乙烯45质量份,含氯量23wt%的氯化聚乙烯48质量份,十八烷基聚苯乙烯7质量份。
十八烷基聚苯乙烯制备时使用十八醇代替正辛醇,其他同实施例1。
实施例3
功能母粒由以下组分在230℃下挤出造粒制得:熔体流动速率MFR为140g/10分钟、密度为0.963g/cm3的聚乙烯55质量份,含氯量27wt%的氯化聚乙烯32质量份,三十烷基聚甲基丙烯酸甲酯13质量份。
三十烷基聚甲基丙烯酸甲酯的制备:首先按公开的合成方法(高等学校化学学报2008年29卷第2期404页)制备α-羧基二硫代苯甲酸丙酯。
将5gα-羧基二硫代苯甲酸丙酯加入到烧瓶中,再加入提纯后的二氯甲烷25mL,搅拌溶解得澄清溶液后用注射器取10mL提纯过的二氯亚砜搅拌条件下加到烧瓶中,然后加热到60℃,回流2h,冷却,静置过夜。减压抽取过量的二氯亚砜,静置过夜。
将2mmol三十烷醇、80mL提纯后的二氯甲烷加入烧瓶中,搅拌溶解后加入1mL干燥的无水吡啶,用20mL提纯的二氯甲烷溶解酰氯化的α-羧基二硫代苯甲酸丙酯,滴加到烧瓶中,室温下避光反应12h。加入无水碳酸钠静置2h除去反应产生的HCl,过滤。将滤液浓缩,用冰甲醇沉淀,过滤,用甲醇洗涤,最后将过滤产物α-三十烷基酯基二硫代苯甲酸丙酯置于真空烘箱中常温下干燥12h备用。
在聚合管中依次加入7mgα-三十烷基酯基二硫代苯甲酸丙酯、1mg偶氮二异丁腈、53ml甲基丙烯酸甲酯、10ml丙酮,均匀混合后用液氮冷却-抽真空-通氮-解冻重复3次,真空封管,于80℃搅拌10h。粗产物在甲醇/水(v/v:1/1)中沉淀,干燥后得到三十烷基聚甲基丙烯酸甲酯。
实施例4
功能母粒由以下组分在210℃下挤出造粒制得:熔体流动速率MFR为200g/10分钟、密度为0.956g/cm3的聚乙烯58质量份,含氯量22wt%的氯化聚乙烯39质量份,十二烷基聚丙烯酸丁酯3质量份。
十二烷基聚丙烯酸丁酯的制备:在聚合管中依次加入3mg 2-氰基-2-丙基十二烷基三硫代碳酸酯、1.6mg过氧化二苯甲酰、34ml丙烯酸丁酯、6ml丙酮,均匀混合后用液氮冷却-抽真空-通氮-解冻重复3次,真空封管,于70℃搅拌12h。粗产物在甲醇/水(v/v:1/1)中沉淀,干燥后得到十二烷基聚丙烯酸丁酯。
实施例5
功能母粒由以下组分在240℃下挤出造粒制得:熔体流动速率MFR)260g/10分钟、密度为0.965g/cm3的聚乙烯41质量份,含氯量24wt%的氯化聚乙烯50质量份,十六烷基聚甲基丙烯酸甲酯9质量份。
十六烷基聚甲基丙烯酸甲酯室温制备:在安瓿瓶中依次加入6.4mg溴十六烷、3.0mg CuBr、3.3mg bpy(联吡啶)和120ml甲基丙烯酸甲酯,通过三次冷冻-抽气-解冻循环过程除氧,随后密封置于90℃油浴中反应。反应进行12小时后取出安瓿瓶,并将其投入液氮中,终止反应。产物用四氢呋喃溶解稀释后,通过中性氧化铝柱子除去金属催化剂。所得滤液浓缩后在甲醇/水(v/v:1/1)中沉淀,所得产物在50℃下真空干燥得到十六烷基聚甲基丙烯酸甲酯。
实施例6
功能母粒由以下组分在180℃下挤出造粒制得:熔体流动速率MFR为180g/10分钟、密度为0.963g/cm3的聚乙烯52质量份,含氯量26wt%的氯化聚乙烯40质量份,十烷基聚丙烯酸甲酯8质量份。
实施例7
功能母粒由以下组分在170℃下挤出造粒制得:熔体流动速率MFR为260g/10分钟、密度为0.965g/cm3的聚乙烯41质量份,含氯量34wt%的氯化聚乙烯50质量份,十六烷基聚甲基丙烯酸甲酯9质量份。
对比例1
功能母粒的组分中不含辛烷基聚苯乙烯,其他组分同实施例1。
对比例2
功能母粒组分中不含氯化聚乙烯,其他组分同实施例2。
对比例3
功能母粒组分中不含聚乙烯,其他组分同实施例3。
对比例4
功能母粒由以下组分在210℃下挤出造粒制得:熔体流动速率MFR为10g/10分钟、密度为0.990g/cm3的聚乙烯58质量份,含氯量22wt%的氯化聚乙烯39质量份,十二烷基聚丙烯酸丁酯3质量份。
对比例5
功能母粒由以下组分在240℃下挤出造粒制得:熔体流动速率MFR为180g/10分钟、密度为0.963g/cm3的聚乙烯52质量份,含氯量26wt%的氯化聚乙烯40质量份,聚丙烯酸甲酯8质量份。
试验例1
实施例1~7和对比例1~5所制得的母料在聚乙烯中的应用对比。
分别向高密度聚乙烯树脂HDPE(兰州石化公司产品8008,熔体流动速率7.0g/10min,密度0.956g/cm3)、线性低密度聚乙烯树脂LLDPE(兰州石化公司产品7042,熔体流动速率2.0g/10min,密度0.918g/cm3)中添加一定质量百分比的实施例的功能母粒得到改性的聚乙烯树脂,并制成测试所需的试验样件,添加对比例的功能母粒或者未添加功能母粒的聚乙烯树脂制备的试验样件为对比样。对试验样和对比样进行性能测试,测试结果如表1所示。
表1加入实施例、对比例母料和加入前后聚乙烯树脂性能对比
从表1中试验样1~7数据和对比样6、7可知,在聚乙烯树脂中添加满足本发明要求的功能母粒,可以在保持基体树脂力学性能基本不变或者有所提高的前提下,提高维卡软化温度10℃(基体树脂为高密度聚乙烯树脂)或15℃(基体树脂为低密度聚乙烯树脂)以上。
从表1中对比样1~4数据可知,若功能母粒中缺少本发明中的某一组分,或所用组分(A)中聚乙烯的熔体流动速率MFR不在本发明限定的范围内,不具有明显提升产品耐热性能的效果,且有可能对某方面的力学性能造成不利影响。
从表1中对比样5数据可知,母粒中用聚丙烯酸酯代替组分(C)不能起到提高树脂组合物耐热性能的效果。
综上所述,本发明公开的聚乙烯功能母粒中,由于聚乙烯(A)、氯化聚乙烯(B)和聚合物(C)三组分共同存在,使得组分(A)能够形成完善的晶区,组分(C)中的极性基团R2与组分(B)氯化聚乙烯的氯原子由于极性协同相互作用形成以氯化聚乙烯为内层,极性基团R2为中间层,长链烷基R1为外层的复合结构。长链烷基R1分散于聚乙烯中提高了组分(B)、(C)和聚乙烯的相容性。最终形成聚乙烯晶区被组分(B)、(C)组装聚集体贯穿的双连续相结构,组分(B)、(C)组装的聚集体形成了晶区之间的联结,在受热时由于晶区和晶区之间有较强的分子链连接,从而不易断裂,提高了聚乙烯功能母粒的耐热性能。
本发明所公开的树脂组合物,由于功能母粒通过三种组分的协同作用起到提升树脂组合物耐热性能的作用,因此采取先制备功能母粒,再与聚乙烯树脂掺混的方法相比直接在聚乙烯树脂中加入各组分具有分散效果更好使树脂组合物性能更加均匀的优点。
与现有技术相比,本发明不需要加入大量的无机物,得到的功能母粒添加到聚乙烯树脂中可有效提升聚乙烯树脂的耐热性,而且添加后的聚乙烯树脂性能均匀稳定。
当然,本发明还可有其它多种实施例,在不背离本发明精神及其实质的情况下,熟悉本领域的技术人员可根据本发明作出各种相应的改变和变形,但这些相应的改变和变形都应属于本发明的保护范围。
Claims (9)
1.一种聚乙烯功能母粒,其特征在于,以聚乙烯功能母粒为100质量份计,由以下组分制备而成:
(A)聚乙烯40~60质量份;
(B)氯化聚乙烯30~50质量份;
(C)包含式(I)所示结构单元的聚合物1~15质量份;
其中,R1为含有8~32个碳原子的烷基;R2为C6H5或COOR,R为正丁基、甲基或叔丁基,R3为H或CH3;3≤n≤100;
其中,所述组分(A)聚乙烯为乙烯均聚物,在温度190℃、负荷2.16Kg下的熔体流动速率MFR为20~300g/10分钟,密度≥0.955g/cm3;
所述氯化聚乙烯中氯元素的含量为氯化聚乙烯总质量的20wt%~30wt%。
2.根据权利要求1所述的聚乙烯功能母粒,其特征在于,所述组分(A)用量为43~55质量份。
3.根据权利要求1所述的聚乙烯功能母粒,其特征在于,所述R1选自正辛烷基、正癸烷基、正十二烷基、十四烷基、十六烷基、十八烷基、二十烷基、二十二烷基、二十四烷基、二十六烷基、二十八烷基、三十烷基、三十二烷基中一种。
4.根据权利要求1所述的聚乙烯功能母粒,其特征在于,所述5≤n≤50。
5.根据权利要求4所述的聚乙烯功能母粒,其特征在于,所述组分(C)聚合物包含结构单元:-(CH2)14-b-(St)80-、-(CH2)20-b-(nBA)60-、-(CH2)30-b-(MMA)30-或-(CH2)24-b-(tBA)40-,其中,St为苯乙烯,nBA为丙烯酸正丁酯,MMA为甲基丙烯酸甲酯,tBA为丙烯酸叔丁酯。
6.根据权利要求1所述的聚乙烯功能母粒,其特征在于,所述氯化聚乙烯中氯元素的含量为氯化聚乙烯总质量的21wt%~25wt%。
7.根据权利要求1所述的聚乙烯功能母粒,其特征在于,所述组分(A)聚乙烯的密度≥0.958g/cm3。
8.一种权利要求1-7任一项所述的聚乙烯功能母粒的制备方法,其特征在于,将组分(A)聚乙烯、组分(B)氯化聚乙烯和组分(C)聚合物在160℃-290℃下挤出造粒后得到该聚乙烯功能母粒。
9.一种树脂组合物,其特征在于,由以下组分制备而成:
(N)聚乙烯;
(M)权利要求1-5任一项所述的聚乙烯功能母粒,
其中,以组分(N)聚乙烯的质量为100%计,组分(M)聚乙烯功能母粒的含量为5wt%~20wt%;组分(N)聚乙烯选自HDPE、LLDPE、LDPE中的至少一种。
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