CN112888737B - 挤出发泡的聚合组合物和制备挤出发泡的聚合组合物的方法 - Google Patents
挤出发泡的聚合组合物和制备挤出发泡的聚合组合物的方法 Download PDFInfo
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- CN112888737B CN112888737B CN201880098940.5A CN201880098940A CN112888737B CN 112888737 B CN112888737 B CN 112888737B CN 201880098940 A CN201880098940 A CN 201880098940A CN 112888737 B CN112888737 B CN 112888737B
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- ethylene
- extrusion
- polymeric composition
- olefin
- polymer
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Classifications
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0012—Combinations of extrusion moulding with other shaping operations combined with shaping by internal pressure generated in the material, e.g. foaming
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
含有挤出发泡的聚合组合物的制品。所述挤出发泡的聚合组合物含有基于乙烯的聚合物和基于烯烃的弹性体。所述挤出发泡的聚合组合物可以由含有所述基于乙烯的聚合物、所述基于烯烃的弹性体、成核剂和起泡剂的可发泡聚合组合物制备。可以使用挤出发泡工艺来制备所述挤出发泡的聚合组合物。
Description
技术领域
本公开的各种实施例涉及包含挤出发泡的聚合组合物的制品。其他方面涉及用于挤出发泡聚合化合物的工艺。
发明内容
一个实施例是一种制品,其包含:
挤出发泡的聚合组合物,所述挤出发泡的聚合组合物包含基于乙烯的聚合物和基于烯烃的弹性体;并且
其中基于乙烯的聚合物的密度为至少0.91g/cm3,
其中弹性体的密度小于0.91g/cm3,
其中挤出发泡的聚合组合物的发泡率为至少20%,
其中挤出发泡的聚合组合物在0℃下的DMA储能模量小于130MPa。
另一个实施例是一种制备挤出发泡的聚合物组合物的方法,该方法包含:
将基于乙烯的聚合物、基于烯烃的弹性体、成核剂和起泡剂合并,以形成可发泡聚合组合物,
通过挤出机挤出至少一部分的可发泡聚合组合物,从而形成挤出发泡的聚合组合物,
其中挤出步骤以至少每分钟1米的线速度进行,
其中基于乙烯的聚合物的密度为至少0.91g/cm3,
其中弹性体的密度小于0.91g/cm3,
其中挤出发泡的聚合组合物的发泡率为至少20%。
具体实施方式
如上所指出,本公开的各种实施例涉及包含基于乙烯的聚合物和基于烯烃的弹性体的挤出发泡的聚合组合物。挤出发泡的聚合组合物通过挤出发泡工艺由包含基于乙烯的聚合物、基于烯烃的弹性体、成核剂和起泡剂的可发泡聚合组合物制备。任选地,可发泡聚合组合物和所得的挤出发泡的聚合组合物可含有一种或多种添加剂。
基于乙烯的聚合物
如上所指出,本文所述的挤出发泡的聚合组合物的一种组分是基于乙烯的聚合物。如本文中所使用,“基于乙烯的”聚合物为由作为主要(即大于50重量%(“wt%”))单体组分的乙烯单体制备的聚合物,但也可以采用其它共单体。“聚合物”意味着通过使相同或不同类型的单体反应(即聚合)而制备的大分子化合物,并且包括均聚物和互聚物。“互聚物”意味着通过至少两种不同单体类型的聚合而制备的聚合物。此通用术语包括共聚物(通常用于指由两种不同单体类型制备的聚合物)和由多于两种不同单体类型制备的聚合物(例如,三元共聚物(三种不同单体类型)和四元共聚物(四种不同单体类型))。
在各种实施例中,基于乙烯的聚合物可为乙烯均聚物。如本文中所使用,“均聚物”表示包含衍生自单个单体类型的重复单元的聚合物,但不排除残余量的用于制备所述均聚物的其它组分,所述均聚物如链转移剂。
在一个或多个实施例中,按全部互聚物重量计,基于乙烯的聚合物可为具有至少1wt%、至少5wt%、至少10wt%、至少15wt%、至少20wt%或至少25wt%的α-烯烃含量的乙烯/α-烯烃(“α烯烃”)互聚物。按全部互聚物重量计,这些互聚物可具有小于50wt%、小于45wt%、小于40wt%或小于35wt%的α-烯烃含量。当采用α-烯烃时,α-烯烃可为C3-20(即具有3至20个碳原子)的直链、支链或环状α-烯烃。C3-20α-烯烃的实例包括丙烯、1丁烯、4-甲基-1-戊烯、1-己烯、1-辛烯、1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯和1-十八碳烯。α-烯烃还可具有环状结构,如环己烷或环戊烷,产生如3-环己基-1-丙烯(烯丙基环己烷)和乙烯基环己烷的α-烯烃。说明性乙烯/α-烯烃互聚物包括乙烯/丙烯、乙烯/1-丁烯、乙烯/1-己烯、乙烯/1-辛烯、乙烯/丙烯/1-辛烯、乙烯/丙烯/1-丁烯和乙烯/1-丁烯/1-辛烯。
在各种实施例中,基于乙烯的聚合物可单独使用或与一种或多种其它类型的基于乙烯的聚合物(例如单体组成和含量、制备的催化方法等方面彼此不同的两种或更多种基于乙烯的聚合物的共混物)组合使用。如果采用基于乙烯的聚合物的共混物,则可通过任何反应器内或后反应器工艺来共混聚合物。
在实施例中,基于乙烯的聚合物可以为低密度聚乙烯(“LDPE”)。LDPE一般为高度支化的乙烯均聚物,并且可通过高压工艺来制备(即,HP-LDPE)。适用于本文中的LDPE可具有0.91至0.94g/cm3范围内的密度。在各种实施例中,基于乙烯的聚合物为密度为至少0.91g/cm3,但小于0.94g/cm3或小于0.93g/cm3的高压LDPE。本文所提供的聚合物密度根据ASTM国际(“ASTM”)方法D792测定。适用于本文中的LDPE的熔体指数(I2)可小于20g/10min,或在0.1至10g/10min、0.5至5g/10min、1至3g/10min范围内,或者I2为2g/10min。本文提供的熔体指数根据ASTM方法D1238测定。除非另外指出,否则熔体指数在190℃和2.16Kg(即I2)下测定。一般来说,LDPE具有宽分子量分布(“MWD”),产生相对高的多分散指数(“PDI”;重均分子量与数均分子量的比)。
在实施例中,基于乙烯的聚合物可以为线性低密度聚乙烯(“LLDPE”)。LLDPE通常是具有非均匀分布的共聚单体(例如,α-烯烃单体)的基于乙烯的聚合物,并且其特征在于短链支化。例如,LLDPE可以为乙烯和如上文所描述的那些α-烯烃单体的共聚物。适用于本文中的LLDPE可具有0.916至0.925g/cm3范围内的密度。适用于本文中的LLDPE可具有1至20g/10min或3至8g/10min范围内的熔体指数(I2)。
用于制备基于乙烯的聚合物的生产工艺是广泛的、变化的并且本领域中已知的。用于生产具有上文所描述特性的基于乙烯的聚合物的任何常规或下文所发现的生产工艺都可用于制备本文所描述的基于乙烯的聚合物。一般来说,聚合可在本领域中已知用于齐格勒-纳塔(Ziegler-Natta)或卡明斯基-辛(Kaminsky-Sinn)型聚合反应的条件下实现,即,在0℃至250℃或30℃或200℃的温度下并且在大气压至10,000大气压(1,013兆帕斯卡(“MPa”))的压力下实现。在大多数聚合反应中,所采用的催化剂与可聚合化合物的摩尔比为10-12:1至10-1:1,或10-9:1至10-5:1。
在一个或多个实施例中,基于乙烯的聚合物是低密度聚乙烯均聚物,其密度为至少0.91g/cm3或在0.91至0.93g/cm3、0.915至0.925g/cm3的范围内,或为约0.92g/cm3。另外,低密度聚乙烯的熔体指数(I2)可在0.1至10g/10min、0.2至9g/10min或0.25至8g/10min范围内。
合适的可商购的基于乙烯的聚合物的实例包括但不限于DOWTM LDPE 132I,可从美国密歇根州米德兰市(Midland,MI,USA)的陶氏化学公司(The Dow Chemical Company)商购获得;DOW AXELERONTMCX 1253NT CPD,可从美国密歇根州米德兰市的陶氏化学公司商购获得;和DOW AXELERONTMCX 1258NT CPD,可从美国密歇根州米德兰市的陶氏化学公司商购获得。
基于烯烃的弹性体
如上所指出,挤出发泡的聚合组合物包含基于烯烃的弹性体。基于烯烃的弹性体包括聚烯烃均聚物和互聚物。聚烯烃互聚物的实例是乙烯/α-烯烃互聚物和丙烯/α-烯烃互聚物。在这类实施例中,α-烯烃可为C3-20直链、支链或环状α-烯烃(对于丙烯/α-烯烃互聚物,乙烯被认为是α-烯烃)。C3-20α-烯烃的实例包括丙烯、1-丁烯、4-甲基-1-戊烯、1-己烯、1-辛烯、1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯和1-十八碳烯。α-烯烃还可含有环状结构,如环己烷或环戊烷,产生如3-环己基-1-丙烯(烯丙基环己烷)和乙烯基环己烷的α-烯烃。尽管不是在该术语的传统意义上的α-烯烃,但是对于本发明的目的,某些环烯烃,如降冰片烯和相关的烯烃,是α-烯烃,并且可以用于代替一些或所有如上所述的α-烯烃。类似地,苯乙烯及其相关的烯烃(例如,α-甲基苯乙烯等)是用于本公开的目的的α-烯烃。说明性聚烯烃共聚物包括乙烯/丙烯、乙烯/丁烯、乙烯/1-己烯、乙烯/1-辛烯、乙烯/苯乙烯等。说明性三元共聚物包括乙烯/丙烯/1-辛烯、乙烯/丙烯/丁烯、乙烯/丁烯/1-辛烯和乙烯/丁烯/苯乙烯。互聚物可以是无规的或嵌段的。
基于烯烃的弹性体也可包含一个或多个官能团,如不饱和酯或酸或硅烷,并且这些弹性体是众所周知的并且可通过常规高压技术而制备。不饱和酯可为丙烯酸烷基酯、甲基丙烯酸烷基酯或羧酸乙烯基酯。烷基可具有1至8个碳原子,并且优选具有1至4个碳原子。羧酸酯基团可具有2至8个碳原子,并且优选具有2至5个碳原子。按共聚物的重量计,归因于酯共聚单体的共聚物的部分可在1至高达50重量%范围内。丙烯酸酯和甲基丙烯酸酯的实例是丙烯酸乙酯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸叔丁酯、丙烯酸正丁酯、甲基丙烯酸正丁酯和丙烯酸2-乙基己酯。羧酸乙烯酯的实例是乙酸乙烯酯、丙酸乙烯酯和丁酸乙烯酯。不饱和酸的实例包括丙烯酸或马来酸。不饱和硅烷的一个实例是乙烯基三烷氧基硅烷。
官能团也可通过接枝包括在基于烯烃的弹性体中,这可按照本领域公知的方法完成。在一个实施例中,接枝可通过自由基官能化的方式发生,所述自由基官能化通常包括将烯烃聚合物、自由基引发剂(如过氧化物等)和含有官能团的化合物熔融共混。在熔融共混期间,自由基引发剂与烯烃聚合物反应(反应性熔融共混)以形成聚合物自由基。含有官能团的化合物键合到聚合物自由基的主链上以形成官能化的聚合物。含有官能团的示例性化合物包括但不限于烷氧基硅烷(例如乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷)和乙烯基羧酸和酸酐(例如马来酸酐)。
适用于本文中的基于烯烃的弹性体的密度可以为小于0.91g/cm3,或在0.85至0.90g/cm3、0.85至0.88g/cm3、或0.855至0.875g/cm3的范围内。另外,基于烯烃的弹性体的熔体指数(I2)可以在0.5至10g/10min或0.7至5.0g/10min的范围内。
可用于本文的基于烯烃的弹性体的更具体的实例包括极低密度聚乙烯(“VLDPE”)(例如,陶氏化学公司制造的FLEXOMERTM乙烯/1-己烯聚乙烯)、均相支化的线性乙烯/α-烯烃共聚物(例如三井石油化学有限公司(Mitsui Petrochemicals Company Limited)的TAFMERTM和埃克森化学公司(Exxon Chemical Company)的EXACTTM),以及均相支化的基本线性的乙烯/α-烯烃聚合物(例如,购自陶氏化学公司的AFFINITYTM和ENGAGETM聚乙烯)。适合使用的ENGAGETM弹性体的具体实例包括但不限于ENGAGETM 8207、ENGAGETM 7447和ENGAGETM 8842,它们均购自陶氏化学公司。
可用于本文的基于烯烃的弹性体还包括丙烯、丁烯和其他基于烯烃的共聚物,例如,包含大部分衍生自丙烯的单元和少量衍生自另一种α-烯烃(包括乙烯)的单元的共聚物。可用于本文的示例性丙烯聚合物包括购自陶氏化学公司的VERSIFYTM聚合物和购自埃克森美孚化学公司(ExxonMobil Chemical Company)的VISTAMAXXTM聚合物。
基于烯烃的弹性体还可包括乙烯-丙烯-二烯单体(“EPDM”)弹性体和氯化聚乙烯(“CPE”)。合适的EPDM的商业实例包括购自陶氏化学公司的NORDELTM EPDM。适合使用的EPDM的具体实例是购自陶氏化学公司的NORDELTM IP 3722P EL。
其他合适的基于烯烃的弹性体包括烯烃嵌段共聚物(如以商品名INFUSETM从美国密歇根州米德兰市的陶氏化学公司商购的那些)、中间相分离的烯烃多嵌段互聚物(如美国专利第7,947,793号中所述)和烯烃嵌段复合物(如美国专利第8,822,598号、第8,686,087号和第8,716,400号;以及PCT公开申请第WO 2017/044547号和第WO 2014/043522号中所述的那些)。
适用于本文中的可商购的烯烃嵌段共聚物的实例包括但不限于购自美国密歇根州米德兰市的陶氏化学公司的INFUSETM 9107。
成核剂
如上所指出,挤出发泡的聚合组合物可以由含有成核剂的可发泡聚合组合物制备。“成核剂(nucleator)”或“成核剂(nucleating agent)”是通常为小颗粒的物质,其为聚合物熔体中的气泡形成提供成核位点或位置。成核剂用于增强发泡的聚合物的泡孔结构。合适的成核剂的非限制性实例包括氟树脂、氮化硼、氧化铝、二氧化硅、聚(4-甲基戊烯)、氧化锆、滑石、偶氮二甲酰胺(“ADCA”)和4,4'-氧双苯磺酰肼(“OBSH”)。在实施例中,成核剂选自氟树脂、氮化硼、ADCA、二氧化硅、聚(4-甲基戊烯)及其组合或两种或更多种。在各种实施例中,成核剂是ADCA。
氟树脂可以是各种聚合物,包括含氟单体的均聚物和共聚物。合适的氟树脂的非限制性实例包括聚四氟乙烯(“PTFE”)、四氟乙烯-全氟烷基乙烯基醚共聚物(“PFA”)、乙烯四氟乙烯共聚物(“ETFE”)、四氟乙烯-六氟丙烯共聚物(“FEP”)、四氟乙烯-乙烯共聚物、聚偏二氟乙烯(“PVdF”)、聚氯三氟乙烯(“PCTFE”)、氯三氟乙烯-乙烯共聚物(“ECTFE”)等。在实施例中,成核剂是选自PTFE、PFA、ETFE及其组合的氟树脂。在另一个实施例中,成核剂是PTFE。
在各种实施例中,成核剂可以作为包括成核剂和聚合组分(例如LDPE)的成核母料掺入到可发泡聚合组合物中。商业成核母料的实例包括购自美国密歇根州米德兰市的陶氏化学公司的AXELERONTM CX A-0012NT CPD。
起泡剂
在实施例中,使用起泡剂制备挤出发泡的聚合组合物。起泡剂是一种或多种适合于挤出温度、发泡条件、泡沫形成方法等。合适的起泡剂包括,例如,惰性气体,如氮气、碳气体(例如,CO、CO2等)、氦气、氩气等;烃、如甲烷、丙烷、丁烷、戊烷等;和卤代烃、如二氯二氟甲烷、二氯一氟甲烷、一氯二氟甲烷、三氯一氟甲烷、一氯五氟乙烷、三氯三氟乙烷等。
添加剂
在实施例中,挤出发泡的聚合组合物包括一种或多种添加剂。代表性添加剂包括但不限于加工助剂、润滑剂、稳定剂(抗氧化剂)、发泡助剂、表面活性剂、助流剂、粘度控制剂、着色剂、铜抑制剂等。这些添加剂可在加工之前或期间添加到基于乙烯的聚合物和基于烯烃的弹性体中。组合物中任何特定添加剂的量通常为0.01至1wt%,更通常为0.01至0.5wt%,并且甚至更通常为0.01至0.3wt%,并且如果存在的话,按组合物的总重量计,所组合物中添加剂的总量通常为0.01至5wt%,更通常为0.01至2wt%,并且甚至更通常为0.01至1wt%。
可发泡聚合组合物
如上所指出,挤出发泡的聚合组合物可以由含有基于乙烯的聚合物、基于烯烃的弹性体、成核剂、起泡剂和任选地一种或多种添加剂的可发泡聚合组合物制备。
按可发泡聚合组合物或挤出发泡的聚合组合物的总重量计,可发泡聚合组合物以及挤出发泡的聚合组合物分别可以含有量在10至90wt%、20至80wt%或30至70wt%范围内的基于乙烯的聚合物。在一些实施例中,按可发泡聚合组合物或挤出发泡的聚合组合物的总重量计,基于乙烯的聚合物可以以在30至50wt%范围内的量分别存在于可发泡聚合组合物以及挤出发泡的聚合组合物中。
按可发泡聚合组合物或挤出发泡的聚合组合物的总重量计,可发泡聚合组合物以及挤出发泡的聚合组合物分别可以含有量在10至90wt%、20至80wt%或30至70wt%范围内的基于烯烃的弹性体。在一些实施例中,按可发泡聚合组合物或挤出发泡的聚合组合物的总重量计,基于烯烃的弹性体可以以在50至70wt%范围内的量分别存在于可发泡聚合组合物以及挤出发泡的聚合组合物中。
基于乙烯的聚合物和基于烯烃的弹性体的组合重量可以分别占整个可发泡聚合组合物或挤出发泡的聚合组合物的至少50、至少55、至少60、至少65、至少70、至少75、至少80、至少85、至少90或至少95wt%。
在各种实施例中,基于乙烯的聚合物和基于烯烃的弹性体可以以在9:1至1:9、4:1至1:4或7:3至3:7范围内的重量比(基于乙烯的聚合物与基于烯烃的弹性体)存在于可发泡聚合组合物和挤出发泡的聚合组合物中。在其他实施例中,基于乙烯的聚合物和基于烯烃的弹性体可以以在1:1至3:7范围内的重量比(基于乙烯的聚合物与基于烯烃的弹性体)存在于可发泡聚合组合物和挤出发泡的聚合组合物中。
按可发泡聚合组合物的总重量计,可发泡聚合组合物可以含有量在0.05至1wt%、0.1至0.5wt%或0.2至0.4wt%范围内的成核剂。如果以母料形式存在,则按可发泡聚合组合物的总重量计,可发泡聚合组合物可以含有量在0.5至10wt%、1至5wt%或2至4wt%范围内的成核母料。
可以通过本领域已知或以后发现的任何方法来制备可发泡聚合组合物。例如,可以预共混基于乙烯的聚合物和基于烯烃的弹性体,这可以例如通过挤出机,BUSSTM捏合机等来完成。成核剂可以在制备预混料的同时进行混配,也可以在挤出发泡过程期间添加。成核剂可以纯净地、与一种或多种其它添加剂例如抗氧化剂、泡孔稳定剂等组合、或作为母料的一部分添加。在各种实施例中,可将成核剂与基于乙烯的聚合物和基于烯烃的弹性体混合,以实现成核剂在聚合物共混物中的基本上均匀的分散,并且为此,通常优选分批混合,例如通过使用BUSSTM捏合机,以在挤出机中混合。如果首先在挤出机中将成核剂与基于乙烯的聚合物和基于烯烃的弹性体混合,则通常在注入用于发泡的起泡剂之前将其加入。
待使用的起泡剂的量可变化。在实施例中,每100重量份的可发泡聚合物组合物,起泡剂的存在量为0.001-0.1重量份,或0.005-0.05重量份。起泡剂可以在挤出之前混合,或者可以从形成在挤出机的机筒上的起泡剂供应开口供应到挤出机中。
挤出发泡
可发泡组合物可以使用任何已知的或以后发现的挤出发泡方法通过挤出发泡来发泡。在各种实施例中,挤出发泡工艺可以以至少1米每分钟(“m/min”)或至少1.25m/min的速率进行。挤出速度可以根据所需的发泡产品的应用、工艺和厚度而变化。在各种实施例中,挤出发泡工艺可以以高达1,000m/min或更大的速率进行。
作为非限制性实例,本公开的挤出发泡工艺可以使用配备有气体注入***的单螺杆挤出机进行。首先将(一种或多种)聚合物和成核剂母料馈送到挤出机中。气体(起泡剂)可以沿着挤出机的长度注入到中间部分中。聚合物熔体和注入的气体(起泡剂)首先作为两个独立的相共存。当熔体通过挤出机时,随后发生混合以将气体(起泡剂)溶解到熔体中。可以在挤出机的末端使用静态混合器以达到均匀的温度和熔体流动。在从模头中排出之前,将熔体冷却至合适的温度以进行发泡。发泡挤出设备的实例包括如上所述的单螺杆挤出机或串联的两个单螺杆挤出机,其中在进入第二挤出机以分配和冷却熔体之前,第一挤出机用于在末端注入气体的情况下来熔融聚合物。
挤出发泡的聚合组合物
所得的挤出发泡的聚合组合物的发泡率可为至少20%或至少22%。挤出发泡的聚合组合物的“发泡率”通过以下方程确定:
在各种实施例中,挤出发泡的聚合组合物的发泡率可在10%至60%的范围内或在22%至57%的范围内。
挤出发泡的聚合组合物在0℃下的DMA储能模量小于130Mpa、小于100MPa或小于75MPa。DMA储能模量根据下文测试方法部分中提供的程序来测定。在各种实施例中,挤出发泡的聚合组合物在0℃下的DMA储能模量在10至130Mpa、15至100MPa或20至75Mpa的范围内。
挤出发泡的聚合组合物在23℃下的DMA储能模量可小于71MPa、小于60MPa、小于50MPa或小于41MPa。在各种实施例中,挤出发泡的聚合组合物在23℃下的DMA储能模量在10至71Mpa、15至50MPa或16至41MPa的范围内。
在各种实施例中,挤出发泡的聚合组合物在23℃下的DMA储能模量比非发泡但在其他方面相同的聚合组合物在23℃下的DMA储能模量低至少25%、少至少30%、少至少35%、少至少40%、至少45%或少至少50%。
挤出发泡的聚合组合物的密度可小于0.7g/cm3或小于0.68g/cm3。在各种实施例中,挤出发泡的聚合组合物的密度可在0.35至0.7g/cm3或0.39至0.68g/cm3的范围内。
制品
上述挤出发泡的聚合组合物可以作为各种制品的一部分或全部被包括在内。这类制品包括但不限于鞋类(例如鞋底)、管道和管材、床垫、汽车应用、电线电缆应用(例如电缆绝缘)、建筑物和建筑应用(例如绝缘材料)等。
测试方法
密度
根据ASTM D792测定密度。
熔体指数
据ASTM D1238,条件190℃/2.16kg测量熔体指数或I2,并且以每10分钟洗脱的克数为单位报告。
模量和力学分析
为了进行拉伸、挠曲模量和动态力学分析测试,将组合物压缩模塑成固体(非发泡)板。准备4英寸×4英寸×0.050英寸厚的板。将每种组合物的粒料在低压(500psi)下于125℃压制3分钟,升至高压(2500psi)3分钟,然后在高压下冷却至30℃。将模制板取出,切成片并在相同条件下再次压制。
使用ARES流变仪对固体样品(非发泡)测试动态力学分析(DMA),以评估组合物的模量随温度的变化。DMA测试条件为0.025%应变,温度从-80℃至120℃,以3℃/分钟的速率,1Hz的频率以及3分钟的浸泡时间。类似地,使用ARES流变仪对挤出的泡沫样品测试DMA,以评估组合物的模量随温度的变化。发泡的样品的DMA测试条件为0.025%应变,温度从-50℃至120℃,以3℃/分钟的速率,1Hz的频率以及3分钟的浸泡时间。
在Instru-Met 4201型拉伸试验机上根据ASTM D638塑料拉伸特性标准测试方法,对固体样品(非发泡)进行拉伸和伸长率(T&E)测试。用100磅荷重计,以每分钟20英寸十字头速度、2.5英寸夹爪宽度测试T&E。根据ASTMD638标准,将每个样本切割为标称厚度为0.075英寸的IV型狗骨。
根据非增强和增强塑料及电绝缘材料的挠曲特性的ASTM D790标准测试方法对固体样品(非发泡)测试挠曲模量。
材料
在下文实例中采用以下材料。
DOWTM LDPE 132I是一种低密度聚乙烯,其密度为0.92g/cm3并且熔体指数(I2)为0.25g/10min,可从美国密歇根州米德兰市的陶氏化学公司商购获得。
ENGAGETM 8207是聚烯烃弹性体,其密度为0.870g/cm3并且熔体指数(I2)为5.0g/10min,可从美国密歇根州米德兰市的陶氏化学公司商购获得。
ENGAGETM 7447是聚烯烃弹性体,其密度为0.865g/cm3并且熔体指数(I2)为5.0g/10min,可从美国密歇根州米德兰市的陶氏化学公司商购获得。
ENGAGETM 8842是聚烯烃弹性体,其密度为0.856g/cm3并且熔体指数(I2)为1.0g/10min,可从美国密歇根州米德兰市的陶氏化学公司商购获得。
INFUSETM 9107是烯烃嵌段共聚物,其密度为0.866g/cm3并且熔体指数(I2)为1.0g/10min,可从美国密歇根州米德兰市的陶氏化学公司商购获得。
NORDELTM IP 3722P EL是EPDM,其密度为0.872g/cm3并且熔体指数(I2)为0.7g/10min,可从美国密歇根州米德兰市的陶氏化学公司商购获得。
IRGANOXTM 1010是季戊四醇四[3-[3,5-二叔丁基-4-羟基苯基]丙酸酯,其位阻酚类抗氧化剂,并且可从德国路德维希港(Ludwigshafen,Germany)的BASF商购获得。
AXELERONTM CX A-0012NT CPD是在高压低密度聚乙烯(“HP LDPE”)中含有10重量%的成核剂的成核母料,其可从美国密歇根州米德兰市的陶氏化学公司商购获得。
实例
使用下表1中提供的配方制备八个非发泡本发明样品(S1-S8)和一个非发泡对比例样品(CS1)。组合物在双螺杆挤出机上制备。在将聚合物粒料馈送到双螺杆挤出机中之前对其进行预混合。组合物在约200℃的熔融温度和40磅/小时下混配。根据上文在“测试方法”部分中所述的制备方法,准备样品的样本进行分析。根据上述测试方法,分析S1-S8和CS1的密度、DMA储能模量、挠曲模量和拉伸模量。结果提供在下表1中。
表1-S1-S8和CS1的配方和特性(非发泡)
使用配备有CO2气体注入***的单螺杆挤出生产线,根据表2中的配方,从S1-S8和CS1制备发泡的样品。将CO2注入挤出机的中桶部分中。CO2气体注入流速为1.0ml/min。在泡沫样品的挤出期间加入成核母料。以1.25m/min的线速度和25rpm的螺杆速度挤出泡沫。根据上述测试方法,分析发泡的S1-S8和CS1的密度和DMA储能模量。结果提供在下表2中。
表2-S1-S8和CS1的配方和特性(发泡)
固体(非发泡)样品的组成和测试结果在表1中给出。发泡的样品的组成和测试结果在表2中给出。比较例(CS1)具有>48%的高发泡率,但是具有不期望高的模量。在-40℃和23℃下,非发泡CS1的储能模量分别超过2199MPa和544MPa。
与CS1不同,本发明的样品(S1至S8)表现出足够高的发泡率和低模量之间的平衡。本发明的组合物,特别是共混物,对比CS1,得到>22%的发泡率(对于轻质来说足够低的密度)、在所有温度下超过30%的DMA储能模量降低(在-40℃下<1620MPa,在0℃下<500MPa,在23℃下<285)、超过46%的2%正割挠曲模量降低,以及超过40%的拉伸模量降低,<90MPa(出于改进的柔韧性)。
Claims (9)
1.一种制品,其包含:
挤出发泡的聚合组合物,所述挤出发泡的聚合组合物包含基于乙烯的聚合物和基于烯烃的弹性体;并且
其中所述基于乙烯的聚合物的密度为至少0.91g/cm3,
其中所述弹性体的密度小于0.91g/cm3,
其中所述基于乙烯的聚合物的存在量范围为按所述挤出发泡的聚合组合物的总重量计30至50重量%,其中所述基于烯烃的弹性体的存在量范围为所述挤出发泡的聚合组合物的50至70重量%,
其中所述挤出发泡的聚合组合物的发泡率为至少20%,
其中所述挤出发泡的聚合组合物在0℃的DMA储能模量小于130Mpa,和
其中所述基于乙烯的聚合物是低密度聚乙烯均聚物,其中所述基于烯烃的弹性体选自由乙烯/α-烯烃互聚物、烯烃嵌段共聚物、烯烃嵌段复合物、乙烯-丙烯-二烯单体EPDM及其两种或更多种的组合组成的组。
2.根据权利要求1所述的制品,其中所述基于乙烯的聚合物和所述弹性体的组合重量占所述挤出发泡的聚合组合物的至少70重量%。
3.根据权利要求1所述的制品,其中所述挤出发泡的聚合组合物在23℃下的DMA储能模量比非发泡但其他方面相同的聚合组合物在23℃下的DMA储能模量低至少25%。
4.根据权利要求1所述的制品,其中所述挤出发泡的聚合组合物的密度小于0.7g/cm3。
5.根据权利要求1所述的制品,其中所述挤出发泡的聚合组合物还包含一种或多种选自抗氧化剂、UV稳定剂、抗粘连剂、交联剂、填料和增塑剂的组分。
6.根据权利要求1所述的制品,其中所述基于乙烯的聚合物的熔体指数I2在0.1至10g/10min的范围内并且密度在0.91至0.93g/cm3的范围内,其中所述基于烯烃的弹性体的熔体指数I2在0.5至10g/10min的范围内并且密度在0.85至0.88g/cm3的范围内。
7.一种制备挤出发泡的聚合物组合物的方法,所述方法包含:
将基于乙烯的聚合物、基于烯烃的弹性体、成核剂和起泡剂合并,以形成可发泡聚合组合物,
通过挤出机挤出至少一部分的所述可发泡聚合组合物,从而形成所述挤出发泡的聚合组合物,其在0℃的DMA储能模量小于130Mpa,
其中挤出步骤以至少每分钟1米的线速度进行,
其中所述基于乙烯的聚合物的密度为至少0.91g/cm3,
其中所述弹性体的密度小于0.91g/cm3,
其中所述基于乙烯的聚合物的存在量范围为按所述挤出发泡的聚合组合物的总重量计30至50重量%,其中所述基于烯烃的弹性体的存在量范围为所述挤出发泡的聚合组合物的50至70重量%,
其中所述挤出发泡的聚合组合物的发泡率为至少20%,和
其中所述基于乙烯的聚合物是低密度聚乙烯均聚物,其中所述基于烯烃的弹性体选自由乙烯/α-烯烃互聚物、烯烃嵌段共聚物、烯烃嵌段复合物、乙烯-丙烯-二烯单体EPDM及其两种或更多种的组合组成的组。
8.根据权利要求7所述的方法,其还包含预共混所述基于乙烯的聚合物和所述基于烯烃的弹性体以形成聚合物预共混物,将所述聚合物预共混物的至少一部分馈送到所述挤出机中,以及将所述成核剂和所述起泡剂与安置在所述挤出机中的所述聚合物预混物合并,以形成所述可发泡聚合组合物。
9.根据权利要求7所述的方法,其中所述成核剂选自由以下组成的组:氟树脂、氮化硼、氧化铝、二氧化硅、聚(4-甲基戊烯)、氧化锆、滑石、偶氮二甲酰胺、4,4'-氧双苯磺酰肼及其两种或更多种的组合;其中所述起泡剂是选自由以下组成的组的惰性气体:二氧化碳、氮气、氦气、氩气、甲烷、丙烷、丁烷、戊烷、二氯二氟甲烷、二氯一氟甲烷、一氯二氟甲烷、三氯一氟甲烷、一氯五氟乙烷、三氯三氟乙烷及其两种或更多种的组合。
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