CN102803387B - 半芳族、半结晶共聚酰胺 - Google Patents
半芳族、半结晶共聚酰胺 Download PDFInfo
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- CN102803387B CN102803387B CN201080056051.6A CN201080056051A CN102803387B CN 102803387 B CN102803387 B CN 102803387B CN 201080056051 A CN201080056051 A CN 201080056051A CN 102803387 B CN102803387 B CN 102803387B
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- copolyamide
- acid
- moulding compound
- ester
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- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims abstract description 24
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- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 6
- 125000003118 aryl group Chemical group 0.000 claims abstract description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 3
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- 229920006114 semi-crystalline semi-aromatic polyamide Polymers 0.000 abstract description 3
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- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/265—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from at least two different diamines or at least two different dicarboxylic acids
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Abstract
半芳族、半结晶共聚酰胺模塑组合物,其包含:A)35-100重量%由如下单元构成的共聚酰胺:a1)35-69重量%衍生于六亚甲基二胺和具有8-16个碳原子的芳族二羧酸的单元,a2)31-65重量%衍生于3,3’-二甲基-4,4’-二氨基二环己基甲烷和对苯二甲酸的单元,a3)0-30重量%不同于a1)和a2)的半结晶聚酰胺单元,B)0-65重量%其他添加剂,其中A)和B)的重量百分数之和为100%。
Description
本发明涉及半芳族、半结晶共聚酰胺模塑组合物,其包含:
A)35-100重量%由如下单元构成的共聚酰胺:
a1)35-69重量%衍生于六亚甲基二胺和具有8-16个碳原子的芳族二羧酸的单元,
a2)31-65重量%衍生于3,3’-二甲基-4,4’-二氨基二环己基甲烷和对苯二甲酸的单元,
a3)0-30重量%不同于a1)和a2)的半结晶聚酰胺单元,
B)0-65重量%其他添加剂,
其中A)和B)的重量百分数之和为100%。
本发明进一步涉及本发明的共聚酰胺在生产纤维、箔和任何类型模制品中的用途以及所得模制品。
耐高温聚酰胺(HTPA)大多基于6T(六亚甲基二胺、对苯二甲酸)单元。然而,直链6T具有非常高的熔点且不能在不导致分解下加工。因此,已经开发了意欲避免此的共聚物体系:例如EP-A 299 444(PA6/6T,PA66/6T),EP-A 19 94 075(PA6T/6I/MXD6),EP-A 667 367(6T/6I/脂环族二胺)。
对于PA 6T/6、6T/6I、6T/66和4T/46体系已经***性地研究了熔点随共聚酰胺掺入量的降低[G.Ajroldi,G.Stea,A.Mattiussi,F.Fumagalli,J.Appl.Poly.Sci.1973,17,3187-3197,H.Ludewig,Faserforschung und Textilchemie 1955,6,277;Gaymans等,J.Polym.Sci.A,Chem.1989,27,423-430]。
具有最高玻璃化转变温度和高熔点(无分解)的HTPA对于许多应用的无问题加工是特别需要的。
因此,本发明基于提供具有高TG和高Tm(无分解)的半芳族、半结晶共聚酰胺这一目的。
因此发现了引言中定义的共聚酰胺模塑组合物。从属权利要求给出了优选的实施方案。
本发明的共聚酰胺模塑组合物包含35-100重量%,优选35-95重量%由如下单元构成的共聚酰胺作为组分A):
a1)35-69重量%,优选40-55重量%,尤其是40-52重量%衍生于六亚甲基二胺和具有8-16个碳原子的芳族二羧酸的单元。
合适芳族二羧酸的实例是对苯二甲酸,间苯二甲酸,取代的对苯二甲酸和间苯二甲酸,例如3-叔丁基间苯二甲酸,多核二羧酸,例如4,4’-和3,3’-二苯基二甲酸,邻苯二甲酸,4,4’-和3,3’-二苯基甲烷二甲酸,二苯基砜-4,4’-和3,3’-二甲酸,1,4-或2,6-萘二甲酸或苯氧基对苯二甲酸,特别优选对苯二甲酸。
单元a2)在共聚酰胺A)中的存在量为31-65重量%,优选45-60重量%,尤其是48-60重量%。这些衍生于3,3’-二甲基-4,4’-二氨基二环己基甲烷和对苯二甲酸。
所用二胺的立体异构体组成优选为50-80重量%反式-反式异构体,而剩余的组成由顺式-反式和顺式-顺式异构体构成且顺式-顺式异构体的比例优选小于10重量%。
本发明的共聚酰胺可以包含0-30重量%不同于a1)和a2)的半结晶聚酰胺单元作为单元a3)。
当存在单元a3)时,优选的所得组成如下:
a1)35-55重量%,尤其是40-50重量%
a2)35-60重量%,尤其是35-45重量%
a3)5-25重量%,尤其是10-22重量%。
对于单元a3),不仅可以使用上述芳族羧酸,而且可以使用脂族二羧酸。
优选的脂族二羧酸是带有具有2-20个碳原子,优选4-16个碳原子,非常特别优选6-14个碳原子的线性或支化烷基的那些。
可以使用的二羧酸是具有两个羧酸基团(羧基)的那些或其衍生物。尤其使用的衍生物是上述二羧酸的单-或二-C1-C10烷基酯,优选单-或二-甲基、乙基、正丙基或异丙基酯,相应的二羰基卤,尤其是二羰基氯,还有相应的二羧酸酐。该类化合物的实例是乙烷二酸(草酸),丙烷二酸(丙二酸),丁烷二酸(琥珀酸),戊烷二酸(戊二酸),己烷二酸(己二酸),庚烷二酸(庚二酸),辛烷二酸(辛二酸),壬烷二酸(壬二酸),癸烷二酸(癸二酸),十一烷二酸,十二烷二酸,十三烷二酸(巴西基酸),C32二聚脂肪酸(由Cognis Corp.,USA销售的产品),其甲基酯,实例是乙烷二酸二甲酯、丙烷二酸二甲酯、丁烷二酸二甲酯、戊烷二酸二甲酯、己烷二酸二甲酯、庚烷二酸二甲酯、辛烷二酸二甲酯、壬烷二酸二甲酯、癸烷二酸二甲酯、十一烷二酸二甲酯、十二烷二酸二甲酯、十三烷二酸二甲酯,C32二聚脂肪酸的二甲基酯,其二酰氯,实例是乙二酰氯、丙二酰氯、丁二酰氯、戊二酰氯、己二酰氯、庚二酰氯、辛二酰氯、壬二酰氯、癸二酰氯、十一烷二酰氯、十二烷二酰氯、十三烷二酰氯,C32二聚脂肪酸的二酰氯,还有其酸酐,实例是丁烷二甲酸和十五烷二甲酸,这里优选十四烷二酸(C14),十五烷二酸(C15),十六烷二酸(C16),十七烷二酸(C17),十八烷二酸(C18),1,4-环己烷二酸。
当然还可以使用上述二羧酸的混合物。
其他形成聚酰胺的单体可以衍生于具有4-16个碳原子的脂族或脂环族二胺,或者衍生于氨基羧酸。这里可以提到的合适的这类单体是作为二胺的代表的1,4-丁二胺、1,5-戊二胺、哌嗪、4,4’-二氨基二环己基甲烷、2,3-(4,4’-二氨基二环己基)丙烷或3,3’-二甲基-4,4’-二氨基二环己基甲烷、六亚甲基二胺、1,8-二氨基辛烷、1,9-二氨基壬烷、1,10-二氨基癸烷、1,12-二氨基十二烷、1,13-二氨基十三烷、2,2,4-或2,4,4-三甲基六亚甲基二胺、苯二甲胺和甲基五亚甲基二胺,以及作为氨基羧酸的代表的ω-氨基十一烷酸。
并非穷举的下面列举包括对本发明提到的可能单元a3)以及所包含的单体:
AA/BB聚合物
AA/BB聚合物:
聚酰胺A)可以通过本身已知的方法(例如EP 129 195,US 3,948,862)生产。还可以使用WO 2007/23108中所述的方法,其中将二酸的对应二腈用作该酸的等价物,或者在水存在下直接聚合,例如如DE-A 10313681,EP-A1198491和EP 922065所述。
本发明的聚酰胺优选以对应二胺和游离二羧酸之间的连续或分批水解缩聚反应由水溶液或水溶性次磷酸盐的水溶液(0.05-0.5重量%)生产。使特性粘度(IV)为40-120ml/g(0.5重量%,在浓硫酸中,ISO 307)的所得预聚物在固相或熔体中在挤出机中进行后缩合过程,直到IV达到至少80ml/g,优选100-300ml/g。
作为替换,本发明的共聚酰胺可以由具有单元a1)的聚酰胺和具有单元a2)的聚酰胺经由熔融和在熔体中的氨基转移,尤其是在挤出机中生产。在这里分开引入相应聚酰胺并任选加入催化添加剂和/或促进剂(实例是次磷酸盐化合物、有机亚磷酸酯或有机膦酸酯)。所得共聚酰胺在氨基转移和共聚酰胺形成方法之后具有单一玻璃化转变温度。
共聚酰胺A)的玻璃化转变温度TG优选高于135°C,特别是高于145°C,尤其是150-190°C。
熔点Tm优选低于330°C,尤其是295-325°C。这些参数通常借助DSC(差示扫描量热法)根据ISO 11357-2,3和7(20K/min,第2加热曲线)测量。
商TG[Kelvin]/Tm[K]优选为至少0.71,尤其是至少0.72,非常特别优选0.73。
本发明的模塑组合物可以包含至多70重量%,优选至多50重量%其他添加剂作为组分B)。
可以提到的纤维状或颗粒状填料是碳纤维、玻璃纤维、玻璃珠、无定形硅石、硅酸钙、偏硅酸钙、碳酸镁、高岭土、白垩、石英粉、云母、硫酸钡和长石,并且这些填料的用量为1-50重量%,尤其是5-40重量%,优选10-40重量%。
可以提到的优选纤维状填料是碳纤维、芳族聚酰胺纤维和钛酸钾纤维,特别优选E玻璃形式的玻璃纤维。这些可以作为粗纱或短切玻璃纤维的市售形式使用。
纤维状填料可能已经用硅烷化合物表面预处理以改进与热塑性材料的相容性。
合适的硅烷化合物具有如下通式:
(X-(CH2)n)k-Si-(O-CmH2m+1)4-k
其中各取代基的定义如下:
n为2-10,优选3-4的整数,
m为1-5,优选1-2的整数,和
k为1-3的整数,优选1。
优选的硅烷化合物是氨基丙基三甲氧基硅烷、氨基丁基三甲氧基硅烷、氨基丙基三乙氧基硅烷和氨基丁基三乙氧基硅烷,以及还有包含缩水甘油基作为取代基X的对应硅烷。
通常用于表面涂敷的硅烷化合物量为0.01-2重量%,优选0.025-1.0重量%,尤其是0.05-0.5重量%(基于B))。
针状矿物填料也是合适的。
对本发明而言,针状矿物填料是具有高度发达的针状特征的矿物填料。实例是针状硅灰石。该矿物优选具有的L/D(长度/直径)比为8:1-35:1,优选8:1-11:1。矿物填料可以任选用上述硅烷化合物预处理,但预处理并不必要。
可以提到的其他填料是高岭土、煅烧高岭土、硅灰石、滑石和白垩,以及还有层状或针状纳米填料,这些的量优选为0.1-10%。对该目的优选的材料是勃姆石、膨润土、蒙脱石、蛭石、锂蒙脱石和锂藻土(laponite)。层状纳米填料通过现有技术方法有机改性,以使它们与有机基料良好相容。在本发明纳米复合材料中加入层状或针状纳米填料使机械强度进一步提高。
本发明的模塑组合物可以包含0.05-3重量%,优选0.1-1.5重量%,尤其是0.1-1重量%润滑剂作为其他组分B)。
优选Al、碱金属或碱土金属的盐,或具有10-44个碳原子,优选12-44个碳原子的脂肪酸的酯或酰胺。
金属离子优选碱土金属和Al,特别优选Ca或Mg。
优选的金属盐是硬脂酸钙和褐煤酸钙,还有硬脂酸铝。
还可以以任何所需混合比使用各种盐的混合物。
羧酸可以是一元或二元的。可以提到的实例是壬酸、棕榈酸、月桂酸、十七烷酸、十二烷二酸、山萮酸,特别优选硬脂酸、癸酸,以及还有褐煤酸(具有30-40个碳原子的脂肪酸混合物)。
脂族醇可以是一元至四元的。醇的实例是正丁醇、正辛醇、硬脂醇、乙二醇、丙二醇、新戊二醇、季戊四醇,优选甘油和季戊四醇。
脂族胺可以是一元至三元的。这些的实例是硬脂胺、乙二胺、丙二胺、六亚甲基二胺、二(6-氨基己基)胺,特别优选乙二胺和六亚甲基二胺。优选的酯或酰胺相应地为甘油二硬脂酸酯、甘油三硬脂酸酯、乙二胺二硬脂酸盐、甘油单棕榈酸酯、甘油三月桂酸酯、甘油单山萮酸酯和季戊四醇四硬脂酸酯。
还可以以任何所需混合比使用各种酯或酰胺的混合物,或者酯与酰胺组合的混合物。
本发明的模塑组合物可以包含0.05-3重量%,优选0.1-1.5重量%,尤其是0.1-1重量%的铜稳定剂,优选卤化铜(I),尤其是与碱金属卤化物,优选KI的混合物,尤其以1:4的比例,或位阻酚或这些的混合物作为其他组分B)。
优选的所用一价铜盐是乙酸亚铜、氯化亚铜、溴化亚铜和碘化亚铜。该材料基于聚酰胺以5-500ppm,优选10-250ppm铜的量包含这些。
若铜以分子分布存在于聚酰胺中,则尤其获得有利的性能。这在将包含聚酰胺、包含一价铜盐且包含碱金属卤化物的浓缩物以固体均相溶液形式加入该模塑组合物中时实现。例如,典型的浓缩物由79-95重量%聚酰胺以及21-5重量%由碘化铜或溴化铜和碘化钾构成的混合物构成。该固体均相溶液中的铜浓度基于该溶液的总重量优选为0.3-3重量%,尤其是0.5-2重量%,且碘化亚铜与碘化钾的摩尔比为1-11.5,优选1-5。
适合该浓缩物的聚酰胺是均聚酰胺和共聚酰胺,尤其是尼龙-6和尼龙-6,6。
合适的位阻酚类B)原则上是所有具有酚类结构且在酚环上具有至少一个庞大基团的化合物。
作为实例,可优选考虑例如下式化合物:
其中R1和R2为烷基、取代的烷基或取代的***基团,并且其中基团R1和R2可以相同或不同,且R3为烷基、取代的烷基、烷氧基或取代的氨基。
上述类型的抗氧化剂例如描述于DE-A 27 02 661(US-A 4 360 617)中。
另一组优选的位阻酚类是衍生于取代的苯羧酸,尤其是取代的苯丙酸的那些。
特别优选的该类化合物是下式化合物:
其中R4、R5、R7和R8相互独立地为本身可以被取代的C1-C8烷基(这些中的至少一个为庞大基团),以及R6为具有1-10个碳原子且其主链还可以具有C-O键的二价脂族基团。
对应于这些式的优选化合物是:
所有下列应作为位阻酚类的实例提及:2,2’-亚甲基二(4-甲基-6-叔丁基苯酚),1,6-己二醇二[3-(3,5-二叔丁基-4-羟基苯基)丙酸酯),季戊四醇四[3-(3,5-二叔丁基-4-羟基苯酚)丙酸酯],3,5-二叔丁基-4-羟基苄基膦酸二硬脂基酯,3,5-二叔丁基-4-羟基氢化肉桂酸2,6,7-三氧杂-1-磷杂双环[2.2.2]辛-4-基甲基酯,3,5-二叔丁基-4-羟基苯基-3,5-二硬脂硫基***基胺,2-(2’-羟基-3’-羟基-3’,5’-二叔丁基苯基)-5-氯苯并***,2,6-二叔丁基-4-羟基甲基苯酚,1,3,5-三甲基-2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯,4,4’-亚甲基二(2,6-二叔丁基苯酚),3,5-二叔丁基-4-羟基苄基二甲基胺。
已经证明特别有效且因此优选使用的化合物是2,2’-亚甲基二(4-甲基-6-叔丁基苯基),1,6-己二醇二(3,5-二叔丁基-4-羟基苯基]丙酸酯(259),季戊四醇四[3-(3,5-二叔丁基-4-羟基苯基)丙酸酯],以及还有N,N’-六亚甲基二-3,5-二叔丁基-4-羟基氢化肉桂酰胺(1098),以及上述BASF SE的产品245,其具有特别好的适用性。
可以单独或作为混合物使用的抗氧化剂B)的含量基于模塑组合物A)-B)的总重量为0.05-3重量%,优选0.1-1.5重量%,尤其是0.1-1重量%。
在某些情形下,已经证明在相对于酚羟基的邻位具有不止一个位阻基团的位阻酚是特别有利的;尤其当评价在散射光中长期储存时的色牢度时。
本发明的模塑组合物可以包含0.05-5重量%,优选0.1-2重量%,尤其是0.25-1.5重量%苯胺黑作为组分B)。
苯胺黑通常为一类与吩嗪蓝相关且呈各种形式(水溶性、油溶性、醇溶性)的黑色或灰色吩嗪染料(吖嗪染料),其用于羊毛染色和羊毛印染,丝绸的染黑以及皮革、鞋油、清漆、塑料、烘漆、油墨等的着色以及还用作显微用染料。
苯胺黑在工业上经由硝基苯、苯胺和苯胺盐酸盐与金属铁和FeCl3的加热而得到(该名称衍生于拉丁语niger=黑色)。
组分B)可以以游离碱或盐(例如盐酸盐)形式使用。
其他常规添加剂B)的实例是至多25重量%,优选至多20重量%的弹性体聚合物(也常称为冲击改性剂、弹性体或橡胶)。
这些非常一般地为优选由下列单体中的至少两种构成的共聚物:乙烯、丙烯、丁二烯、异丁烯、异戊二烯、氯丁二烯、乙酸乙烯酯、苯乙烯、丙烯腈和在醇组分中具有1-18个碳原子的丙烯酸酯和/或甲基丙烯酸酯。
这类聚合物例如描述于Houben-Weyl,Methoden der organischenChemie,第14/1卷(Georg-Thieme-Verlag,Stuttgart,1961),第392-406页以及C.B.Bucknall的单行本,“Toughened Plastics”(Applied SciencePublishers,London,1977)中。
该类弹性体的一些优选类型如下所述。
该类弹性体的优选类型是已知为乙烯-丙烯(EPM)和乙烯-丙烯-二烯烃(EPDM)橡胶的那些。
EPM橡胶通常基本没有残留双键,而EPDM橡胶每100个碳原子可以具有1-20个双键。
可以提到的EPDM橡胶的二烯烃单体实例是共轭二烯烃,如异戊二烯和丁二烯,具有5-25个碳原子的非共轭二烯烃,如1,4-戊二烯,1,4-己二烯,1,5-己二烯,2,5-二甲基-1,5-己二烯和1,4-辛二烯,环状二烯烃,如环戊二烯、环己二烯、环辛二烯和二环戊二烯,以及还有链烯基降冰片烯,如5-亚乙基-2-降冰片烯,5-亚丁基-2-降冰片烯,2-甲代烯丙基-5-降冰片烯和2-异丙烯基-5-降冰片烯,三环二烯类,如3-甲基三环[5.2.1.02,6]-3,8-癸二烯,以及这些的混合物。优选1,5-己二烯,5-亚乙基降冰片烯和二环戊二烯。EPDM橡胶的二烯烃含量基于该橡胶的总重量优选为0.5-50重量%,尤其是1-8重量%。
EPM橡胶和EPDM橡胶还可以优选用反应性羧酸或这些的衍生物接枝。这些的实例是丙烯酸、甲基丙烯酸及其衍生物,例如(甲基)丙烯酸缩水甘油酯,以及还有马来酸酐。
乙烯与丙烯酸和/或甲基丙烯酸和/或与这些酸的酯的共聚物是另一类优选的橡胶。该橡胶还可以包含二羧酸,如马来酸和富马酸,或者这些酸的衍生物,例如酯和酸酐,和/或含环氧基的单体。这些含二羧酸衍生物或含环氧基的单体优选通过向单体混合物中加入含二羧酸基和/或环氧基且具有通式I、II、III或IV的单体而引入橡胶中:
R1C(COOR2)=C(COOR3)R4 (I)
其中R1-R9为氢或具有1-6个碳原子的烷基,m为0-20的整数,g为0-10的整数且p为0-5的整数。
基团R1-R9优选为氢,其中m为0或1且g为1。对应的化合物为马来酸、富马酸、马来酸酐、烯丙基缩水甘油醚和乙烯基缩水甘油醚。
优选的式I、II和IV化合物是马来酸、马来酸酐和含环氧基的(甲基)丙烯酸酯,如丙烯酸缩水甘油酯和甲基丙烯酸缩水甘油酯,以及与叔醇的酯,如丙烯酸叔丁基酯。尽管后者没有游离羧基,但它们的行为接近游离酸且它们因此称为具有潜在羧基的单体。
该共聚物有利地由50-98重量%乙烯、0.1-20重量%含环氧基的单体和/或甲基丙烯酸和/或含酸酐基团的单体、剩余量为(甲基)丙烯酸酯构成。
特别优选由如下单体构成的共聚物:
50-98重量%,尤其是55-95重量%乙烯,
0.1-40重量%,尤其是0.3-20重量%丙烯酸缩水甘油酯和/或甲基丙烯酸缩水甘油酯、(甲基)丙烯酸和/或马来酸酐,和
1-45重量%,尤其是5-40重量%丙烯酸正丁酯和/或丙烯酸2-乙基己基酯。
其他优选的(甲基)丙烯酸酯是甲基、乙基、丙基、异丁基和叔丁基酯。
除了这些以外可以使用的共聚单体是乙烯基酯和乙烯基醚。
上述乙烯共聚物可以通过本身已知的方法,优选在高压和升高的温度下无规共聚而制备。合适的方法是众所周知的。
其他优选的弹性体是其制备例如由Blackley描述于单行本“EmulsionPolymerization”中的乳液聚合物。可以使用的乳化剂和催化剂本身是已知的。
原则上可以使用均相结构的弹性体或具有壳结构的那些。壳型结构由各单体的加入顺序决定。聚合物的形态也受该加入顺序影响。
本文中对于弹性体的橡胶部分的制备仅作为实例可以提到的单体是丙烯酸酯,如丙烯酸正丁酯和丙烯酸2-乙基己基酯,对应的甲基丙烯酸酯,丁二烯和异戊二烯,还有这些的混合物。这些单体可以与其他单体如苯乙烯、丙烯腈、乙烯基醚和其他丙烯酸酯或甲基丙烯酸酯如甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸乙酯或丙烯酸丙酯共聚。
弹性体的软相或橡胶相(玻璃化转变温度低于0°C)可以为核、外壳或中间壳(在其结构具有不止两个壳的弹性体情况下)。具有不止一个壳的弹性体还可以具有不止一个由橡胶相构成的壳。
若除了橡胶相外在弹性体结构中还包含一种或多种硬组分(玻璃化转变温度高于20°C),则这些通常通过聚合作为主单体的苯乙烯、丙烯腈、甲基丙烯腈、α-甲基苯乙烯、对甲基苯乙烯或丙烯酸酯或甲基丙烯酸酯如丙烯酸甲酯、丙烯酸乙酯或甲基丙烯酸甲酯而制备。除了这些以外,还可以使用较小比例的其他共聚单体。
在某些情况下已经证明有利的是使用在其表面具有反应性基团的乳液聚合物。这类基团的实例是环氧基、羧基、潜在羧基、氨基和酰胺基团,以及还有可以通过同时使用如下通式的单体引入的官能团:
其中各取代基可以如下定义:
R10为氢或C1-C4烷基,
R11为氢、C1-C8烷基或芳基,尤其是苯基,
R12为氢、C1-C10烷基、C6-C12芳基或-OR13,
R13为可以任选被包含O的基团或包含N的基团取代的C1-C8烷基或C6-C12芳基,
Y为O-Z或NH-Z,和
Z为C1-C10亚烷基或C6-C12亚芳基。
EP-A 208 187中所述接枝单体也适合在表面引入反应性基团。
可以提到的其他实例是丙烯酰胺、甲基丙烯酰胺和取代的丙烯酸酯或甲基丙烯酸酯,如甲基丙烯酸(N-叔丁基氨基)乙基酯、丙烯酸(N,N-二甲基氨基)乙基酯、丙烯酸(N,N-二甲基氨基)甲基酯和丙烯酸(N,N-二乙基氨基)乙基酯。
橡胶相的颗粒还可以交联。交联单体的实例是1,3-丁二烯、二乙烯基苯、邻苯二甲酸二烯丙基酯和丙烯酸二氢二环戊二烯基酯,以及还有EP-A 50265中所述化合物。
还可以使用已知为接枝连接单体的单体,即具有两个或更多个在聚合过程中以不同速率反应的可聚合双键的单体。优选使用其中至少一个反应性基团与其他单体以大致相同速率聚合,而另一或其他反应性基团例如显著更慢聚合的这类化合物。不同的聚合速率在橡胶中导致一定比例的不饱和双键。此时若在该类橡胶上接枝另一相,则至少一些存在于该橡胶中的双键与接枝单体反应形成化学键,即接枝上的相与接枝基质具有至少一定程度的化学键合。
这类接枝连接单体的实例是含烯丙基的单体,尤其是烯属不饱和羧酸的烯丙基酯,例如丙烯酸烯丙基酯、甲基丙烯酸烯丙基酯、马来酸二烯丙基酯、富马酸二烯丙基酯和衣康酸二烯丙基酯,以及这些二羧酸的对应单烯丙基化合物。除此以外还存在宽范围的其他合适接枝连接单体。其他细节在这里例如可以参考US专利4 148 846。
这些交联单体在冲击改性聚合物中的比例基于冲击改性聚合物通常为至多5重量%,优选不超过3重量%。
一些优选的乳液聚合物列举如下。这里首先可以提到具有核和至少一个外壳且具有下列结构的接枝聚合物:
代替其结构具有不止一个壳的接枝聚合物,还可以使用由1,3-丁二烯、异戊二烯和丙烯酸正丁酯构成的均相,即单一壳弹性体或这些的共聚物。这些产品也可以通过同时使用交联单体或具有反应性基团的单体制备。
优选乳液聚合物的实例是丙烯酸正丁酯-(甲基)丙烯酸共聚物,丙烯酸正丁酯-丙烯酸缩水甘油酯或丙烯酸正丁酯-甲基丙烯酸缩水甘油酯共聚物,具有由丙烯酸正丁酯构成或基于丁二烯的内核且具有由上述共聚物构成的外壳的接枝聚合物以及乙烯与提供反应性基团的共聚单体的共聚物。
所述弹性体还可以通过其他常规方法,例如悬浮聚合制备。
还优选如DE-A 37 25 576,EP-A 235 690,DE-A 38 00 603和EP-A319 290中所述的硅橡胶。
当然还可以使用上述类型橡胶的混合物。
本发明的热塑性模塑组合物可以包含常规加工助剂如稳定剂、氧化抑制剂、对抗热分解和紫外光分解的试剂、润滑剂和脱模剂、着色剂如染料和颜料、成核剂、增塑剂等作为组分B)。
氧化抑制剂和热稳定剂的实例是位阻酚和/或亚磷酸酯和胺(例如TAD),氢醌类,芳族仲胺,如二苯基胺,这些组的各种取代成员,以及这些的混合物,其浓度基于热塑性模塑组合物的重量为至多1重量%。
可以提到的UV稳定剂是各种取代的间苯二酚、水杨酸酯类、苯并***类和二苯甲酮类,其用量基于该模塑组合物通常至多为2重量%。
可以作为着色剂加入的材料是无机颜料,如二氧化钛、群青蓝、氧化铁和碳黑,还有有机颜料,如酞菁、喹吖啶酮类、苝类,以及还有染料如蒽醌类。
可以用作成核剂的材料是苯基次膦酸钠、氧化铝、二氧化硅以及还优选滑石。
本发明的热塑性模塑组合物可以由本身已知的方法通过在常规混合设备,如螺杆基挤出机、Brabender混合机或Banbury混合机中混合起始组分并随后挤出它们而生产。挤出物可以冷却并造粒。还可以预混各组分并随后单独和/或同样以混合物形式加入剩余原料。混合温度通常为230-320°C。
在另一优选程序中,可以将组分B)与预聚物混合、配混并造粒。然后将所得粒料在惰性气体下在低于组分A)的熔点的温度下连续或分批固相缩合,直到达到所需粘度。
本发明的热塑性模塑组合物的特征在于良好的加工性以及良好的机械性能,还有高TG以及高Tm,但聚合物在加工过程中不分解。
这些材料适合生产纤维、箔和任何类型的模制品。一些实例如下:汽缸盖罩、摩托车罩、进气管、增压空气冷却器罩、插接器、齿轮、冷却风扇轮和冷却水箱。
在电气和电子领域中,流动改进的聚酰胺可以用于生产插头,插头部件,插接器,膜开关,印刷电路板组件,微电子组件,线圈,I/0插接器,印刷电路板(PCB)用插头,柔性印刷电路(FPC)用插头,柔性集成电路(FFC)用插头,高速插接器,接线条,连接器插头,器件插头,电缆束组件,电路固定件,电路固定组件,三维注塑电路固定件,电气连接器和机电组件。
在汽车内饰件中的可能应用是用于仪表盘,转向柱开关,座椅组件,靠枕,中控台,变速器组件和门组件,在汽车外饰件中的可能应用是用于门把手,外后视镜组件,挡风玻璃雨刷器组件,挡风玻璃雨刷器保护套,水箱护罩,天窗轨道,天窗框架,发动机罩,汽缸盖罩,进气管(尤其是进气歧管),挡风玻璃雨刷器,以及还有外部车身组件。
流动改进的聚酰胺在厨房和家用领域中的可能应用是用于生产厨房设备如油炸锅的组件,熨斗,旋钮,以及还有在花园和休闲领域中的应用,例如灌溉***的组件,或花园设备,以及门把手。
实施例
将六亚甲基二胺(6)、3,3’-二甲基-4,4’-二氨基二环己基甲烷(L)和对苯二甲酸(T)以及任选还有六亚甲基二胺和己二酸与次磷酸钠单水合物的水溶液(“NHP”;0.1重量%)一起称入测试管中。下表列出了各实施例的混合物中所用合适量。将反应混合物引入高压釜反应器中并吹扫3次,在每种情况下使用3巴的氮气。将该高压釜加热到ET=200°C并在该温度下保持1小时,然后加热到350°C的外部温度,并经由连续减压将16巴的表压维持总共2小时。然后在60分钟内将高压釜减压至环境压力并在相同温度下在氮气流下将缩聚反应进行120分钟。在加压(P=10巴)下冷却该体系,然后将取出的干产物粉碎。
DSC测量:
DSC测量在来自Waters GmbH的Q-2000中进行。
起始重量为约8.5mg且加热和冷却速率为20K/min(第2加热曲线)。
对样本进行的测量基于ISO 11357–2,3和7。
ΔH按如下测定:
计算熔融曲线(第2加热曲线)下的面积
Claims (8)
1.半芳族、半结晶共聚酰胺模塑组合物,其包含:
A)35-100重量%由如下单元构成的共聚酰胺:
a1)35-55重量%衍生于六亚甲基二胺和具有8-16个碳原子的芳族二羧酸的单元,
a2)31-60重量%衍生于3,3’-二甲基-4,4’-二氨基二环己基甲烷和对苯二甲酸的单元,
a3)5-25重量%由六亚甲基二胺和己二酸构成的单元,以及
B)0-65重量%其他添加剂,
其中A)和B)的重量百分数之和为100%。
2.根据权利要求1的共聚酰胺模塑组合物,其中所述共聚酰胺A的TG(玻璃化转变温度)根据ISO11357–2,3和7借助DSC测量为大于135℃。
3.根据权利要求1的共聚酰胺模塑组合物,其中所述共聚酰胺A的熔点Tm根据ISO11357–2,3和7借助DSC测量低于330℃。
4.根据权利要求2的共聚酰胺模塑组合物,其中所述共聚酰胺A的熔点Tm根据ISO11357–2,3和7借助DSC测量低于330℃。
5.根据权利要求1-4中任一项的共聚酰胺模塑组合物,其中所述共聚酰胺A的商TG(K)/Tm(K)为至少0.71。
6.根据权利要求1-4中任一项的共聚酰胺模塑组合物,包含六亚甲基二胺和对苯二甲酸作为单元a1)。
7.根据权利要求1-6中任一项的共聚酰胺模塑组合物在生产纤维、箔和模制品中的用途。
8.一种可以由根据权利要求1-6中任一项的共聚酰胺模塑组合物得到的模制品。
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DE102013218957A1 (de) * | 2013-09-20 | 2015-03-26 | Evonik Industries Ag | Formmasse auf Basis eines teilaromatischen Copolyamids |
DE102013218964A1 (de) * | 2013-09-20 | 2015-03-26 | Evonik Industries Ag | Formmasse auf Basis eines teilaromatischen Copolyamids |
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JP6468783B2 (ja) * | 2014-10-06 | 2019-02-13 | 三菱エンジニアリングプラスチックス株式会社 | ポリアミド樹脂組成物、成形品、および、成形品の製造方法 |
CN109930228B (zh) * | 2017-12-18 | 2022-04-29 | 财团法人纺织产业综合研究所 | 锦纶66改质纤维 |
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CN115667415B (zh) | 2020-05-25 | 2023-12-29 | 菱环球聚甲醛株式会社 | 激光熔敷用透光性树脂组合物、组合物组合、成型品、以及成型品的制造方法 |
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