CN1497015A - 改进的塑料组合物 - Google Patents
改进的塑料组合物 Download PDFInfo
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- CN1497015A CN1497015A CNA03125554XA CN03125554A CN1497015A CN 1497015 A CN1497015 A CN 1497015A CN A03125554X A CNA03125554X A CN A03125554XA CN 03125554 A CN03125554 A CN 03125554A CN 1497015 A CN1497015 A CN 1497015A
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- Prior art keywords
- methyl
- ester
- monomer
- mma
- nano particle
- Prior art date
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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Abstract
一种塑料组合物,包括具有1至100纳米直径的聚合物纳米颗粒和聚合物组分。还提供一种制备这样的塑料组合物的方法。
Description
本发明涉及一种改进的塑料组合物。本发明特别涉及包括具有直径为1至100nm的聚合物纳米颗粒的改进的塑料组合物。与无聚合物纳米颗粒的相同组合物相比,本发明的组合物改进了至少一种性能。本发明还涉及一种提供改进的塑料的方法,包括:形成具有直径为1至100nm的聚合物纳米颗粒;和形成包括聚合物纳米颗粒的塑料组合物。
塑料可单独使用或与其它材料组合形成复合物。由于塑料常常为脆性的或缺少足够强度,因此一直需要提高其机械性能。
聚合物颗粒可用于改进热塑性和热固性树脂的机械性能和熔体加工性能。例如聚氯乙烯树脂和氯化聚氯乙烯树脂(以下统称为“PVC”)具有各种性能的综合,使其特别适合用作结构材料,但仍然存在脆性。PVC与具有橡胶相的聚合物颗粒共混改进了冲击强度(例如作为冲击改性剂)。仍然需要改进可用作塑料添加剂的聚合物颗粒的性能。
WO 200075244公开了通过一种或多种环氧官能粘结剂与具有平均粒度为5至200nm的羧基官能金属-有机纳米颗粒反应形成的粘结剂。
需要提供一种具有至少一种改进性能的塑料组合物。已发现,此改进存在于包括具有直径为1至100nm的聚合物纳米颗粒的塑料组合物中。
本发明的第一方面提供一种包括具有直径为1至100nm的聚合物纳米颗粒的塑料。
本发明第二方面提供一种提供塑料的方法,包括:形成具有直径为1至100nm的聚合物纳米颗粒;和形成包括该聚合物纳米颗粒的塑料组合物。
这里使用的如下简写,除非另有清楚说明,否则将具有如下含义:C=℃;μm=微米;UV=紫外线;rpm=每分钟的转数;nm=纳米;J=焦耳;cc=立方厘米;g=克;wt%=重量百分比;L=升;mL=毫升;pphr=每100份树脂的份数,以重量计;MIAK=甲基异戊基酮;MIBK=甲基异丁基酮;PMA=聚(丙烯酸甲酯);CyHMA=甲基丙烯酸环己酯;EG=乙二醇;DPG=二丙二醇;DFA=乙酸二甘醇乙基醚酯;BzA=丙烯酸苄酯;BzMA=甲基丙烯酸苄酯;MAPS=MATS=甲基丙烯酸(三甲氧基甲硅烷基)丙基酯;PETTA=四/三乙酸季戊四醇酯;PPG4000DMA=二甲基丙烯酸聚丙二醇4000酯;DPEPA=五丙烯酸二季戊四醇酯;TMSMA=甲基丙烯酸三甲基甲硅烷基酯;MOPTSOMS=甲基丙烯酰氧基丙基双(三甲基硅氧烷基)甲基硅烷;MOPMDMOS=3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷;TAT=三烯丙基-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮;IBOMA=甲基丙烯酸异冰片酯;PGMEA=乙酸丙二醇单甲基醚酯,PEGMEMA 475=聚(乙二醇甲基醚)甲基丙烯酸酯Mw=475;GMA=甲基丙烯酸缩水甘油酯;和PGDMA=二甲基丙烯酸丙二醇酯。
术语“(甲基)丙烯酸类”包括丙烯酸和甲基丙烯酸类,术语“(甲基)丙烯酸酯”包括丙烯酸酯和甲基丙烯酸酯。此外,术语“(甲基)丙烯酰胺”是指丙烯酰胺和甲基丙烯酰胺。“烷基”包括直链、支链和环状烷基。
本发明涉及塑料组合物,其包括具有平均粒径为1至100纳米、优选1至50纳米、更优选1至20纳米的聚合物纳米颗粒。PNP进一步通常具有至少1.5nm,优选至少2nm的平均粒径。
测定PNP的颗粒尺寸(平均粒径)的一种方法是使用标准动态光散射技术,其中将相关函数用LaPlace转化法如CONTIN转化为流体力学直径。
通常,PNP具有的玻璃转化温度为-90至170℃(对于聚合的多烯属不饱和单体不存在的组成),通过模态差示扫描量热法测定。
本发明的PNP一般具有“表观重均分子量”在5,000至1,000,000,优选10,000至500,000,更优选15,000至100,000的范围内。这里使用的“表观重均分子量”反映PNP颗粒的尺寸,使用标准凝胶渗透色谱法,例如使用40℃的THF溶剂,3个PlgelTM色谱柱(Polymer Labs,Amherst,MA),100埃(10nm),103埃(100nm),104埃(1微米),30cm长,7.8mm ID,1ml/min,100μl注射体积,用Polymer Lab CALIBRETM的软件校准至窄聚苯乙烯标准。
这里称为聚合物纳米颗粒(“PNP”)的聚合物颗粒为加成聚合物,其含有作为聚合物单元的至少一种多烯属不饱和单体和至少一种烯属不饱和水溶性单体。可用于本发明的合适多烯属不饱和单体包括二-、三-、四-或更高级的多官能烯属不饱和单体,如二乙烯基苯、三乙烯基苯、二乙烯基甲苯、二乙烯基吡啶、二乙烯基萘、二乙烯基二甲苯、二(甲基)丙烯酸乙二醇酯、三羟甲基丙烷三(甲基)丙烯酸酯、二甘醇二乙烯基醚、三乙烯基环己烷、(甲基)丙烯酸烯丙基酯、二(甲基)丙烯酸二甘醇酯、二(甲基)丙烯酸丙二醇酯、2,2-二甲基丙烷-1,3-二(甲基)丙烯酸酯、二(甲基)丙烯酸1,3-丁二醇酯、二(甲基)丙烯酸1,4-丁二醇酯、二(甲基)丙烯酸1,6-己二醇酯、二(甲基)丙烯酸三丙二醇酯、二(甲基)丙烯酸三甘醇酯、二(甲基)丙烯酸四甘醇酯、二(甲基)丙烯酸聚乙二醇酯如二(甲基)丙烯酸聚乙二醇200酯和二(甲基)丙烯酸聚乙二醇600酯、二(甲基)丙烯酸乙氧基化双酚A酯、二(甲基)丙烯酸聚丁二醇酯、三(甲基)丙烯酸季戊四醇酯、三乙氧基三(甲基)丙烯酸三羟甲基丙烷酯、甘油基丙氧基三(甲基)丙烯酸酯、四(甲基)丙烯酸季戊四醇酯、单羟基五(甲基)丙烯酸二季戊四醇酯、二乙烯基硅烷、三乙烯基硅烷、二甲基二乙烯基硅烷、二乙烯基甲基硅烷、甲基三乙烯基硅烷、二苯基二乙烯基硅烷、二乙烯基苯基硅烷、三乙烯基苯基硅烷、二乙烯基甲基苯基硅烷、四乙烯基硅烷、二甲基乙烯基二硅氧烷、聚(甲基乙烯基硅氧烷)、聚(乙烯基氢硅氧烷)、聚(苯基乙烯基硅氧烷)和其混合物。
通常,PNP含至少1wt%的至少一种聚合的多烯属不饱和单体,按PNP重量计。高达并包括99.5wt%的聚合多烯属不饱和单体(按PNP的重量计)有效用于本发明的颗粒中。聚合多烯属不饱和单体的量优选为1至80%、更优选1至60%,最优选1至25%(重量),按PNP的重量计。
可为共聚合单元包括在聚合物纳米颗粒中的合适烯属不饱和单体包括但不限于:(甲基)丙烯酸、(甲基)丙烯酰胺、(甲基)丙烯酸烷基酯、(甲基)丙烯酸链烯基酯、芳族(甲基)丙烯酸酯、乙烯基芳烃单体、含氮的化合物和其含硫类似物和取代的乙烯单体。
PNP任选地包含作为聚合单元的一种或多种不属于多烯属不饱和单体的第三单体。合适的第三单体包括(甲基)丙烯酸C1-C24烷基酯,如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸十二烷基酯、(甲基)丙烯酸十五烷基酯、(甲基)丙烯酸十六烷基酯、(甲基)丙烯酸十八烷基酯和(甲基)丙烯酸十九烷基酯和其混合物。其它合适的第三单体包括(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸1-甲基-2-羟乙基酯、(甲基)丙烯酸2-羟基丁酯、乙酸乙烯酯;维萨酸(versatate)乙烯酯;二异丁烯;乙烯基芳烃单体如苯乙烯、α-甲基苯乙烯、乙烯基甲苯、对-甲基苯乙烯、乙基乙烯基苯、乙烯基萘、乙烯基二甲苯和壬基苯氧基丙烯基聚乙氧基化醇。乙烯基芳烃单体还包括其相应的取代抗衡部分,如卤化衍生物,即含一个或多个卤素基团如氟、氯或溴;和硝基、氰基、(C1-C10)烷氧基、卤代(C1-C10)烷基、(C1-C10)烷氧基、羧基等。
合适的(甲基)丙烯酸烷基酯包括但不限于(甲基)丙烯酸“低级”烷基酯、(甲基)丙烯酸“中级”烷基酯和(甲基)丙烯酸“高级”烷基酯。
(甲基)丙烯酸“低级”烷基酯通常为其中烷基含1至6个碳原子的那些。合适的(甲基)丙烯酸“低级”烷基酯包括但不限于甲基丙烯酸甲酯(“MMA”)、丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯(“BMA”)、丙烯酸丁酯(“BA”)、甲基丙烯酸异丁酯(“IBMA”)、甲基丙烯酸己酯、甲基丙烯酸环己酯和其混合物。
(甲基)丙烯酸“中级”烷基酯通常为其中烷基含7至15个碳原子的那些。合适的(甲基)丙烯酸“中级”烷基酯包括但不限于丙烯酸2-乙基己酯(“EHA”)、甲基丙烯酸2-乙基己酯、甲基丙烯酸辛酯、甲基丙烯酸癸基酯、甲基丙烯酸异癸酯(“IDMA”,基于支化的(C10)烷基异构体混合物)、甲基丙烯酸十一烷基酯、甲基丙烯酸十二烷基酯(又称为甲基丙烯酸月桂酯)、甲基丙烯酸十三烷基酯、甲基丙烯酸十四烷基酯(又称为甲基丙烯酸肉豆蔻基酯)、甲基丙烯酸十五烷基酯和其混合物。可用的混合物包括甲基丙烯酸十二烷基-十五烷基酯(“DPMA”)、甲基丙烯酸十二烷基酯、十三烷基酯、十四烷基酯和十五烷基酯的线性和支化异构体的混合物;以及甲基丙烯酸月桂基-肉豆蔻基酯(“LMA”)。
(甲基)丙烯酸“高级”烷基酯通常为其中烷基含16至24个碳原子的那些。合适的(甲基)丙烯酸”高级”烷基酯包括但不限于甲基丙烯酸十六烷基酯、甲基丙烯酸十七烷基酯、甲基丙烯酸十八烷基酯、甲基丙烯酸十九烷基酯、甲基丙烯酸二十级烷基(cosyl)酯、甲基丙烯酸二十烷基(eicosyl)酯和其混合物。(甲基)丙烯酸“高级”烷基酯的合适混合物包括但不限于:甲基丙烯酸-十六至二十烷基(eicosyl)酯(“CEMA”),它是甲基丙烯酸十六烷基酯、甲基丙烯酸十八烷基酯、甲基丙烯酸二十级烷基(cosyl)酯和甲基丙烯酸二十烷基(eicosyl)酯的混合物;以及甲基丙烯酸十六至十八烷基酯(“SMA”),它是甲基丙烯酸十六烷基酯和十八烷基酯的混合物。
上述(甲基)丙烯酸中级和高级烷基酯单体通常通过使用工业级长链脂族醇的标准酯化工艺制备,这些市购的醇为烷基中含10至15或16至20个碳原子的各种链长度的醇的混合物。这些醇的例子是各种齐格勒催化的ALFOL醇,购自Vista Chemical Company,即ALFOL1618和ALFOL1620,齐格勒催化的各种NEODOL醇,购自Shell Chemical Company,即NEODOL 25L,和天然衍生的醇,如Proctor & Gamble的TA-1618和CO-1270。因此,对于本发明,(甲基)丙烯酸烷基酯不仅包括单一(甲基)丙烯酸烷基酯产品,而且包括具有主要量的特定名称“(甲基)丙烯酸烷基酯”的那些(甲基)丙烯酸烷基酯的混合物。
可用于本发明的(甲基)丙烯酸烷基酯单体可为单一单体或在烷基部分中具有不同碳原子数的混合物。此外,可用于本发明的(甲基)丙烯酰胺和(甲基)丙烯酸烷基酯可任选被取代。合适的任选取代的(甲基)丙烯酰胺和(甲基)丙烯酸烷基酯单体包括但不限于:(甲基)丙烯酸羟基(C2-C6)烷基酯,(甲基)丙烯酸二烷基氨基(C2-C6)烷基酯,二烷基氨基(C2-C6)烷基(甲基)丙烯酰胺。
有用的取代的(甲基)丙烯酸烷基酯单体是在烷基中具有一个或多个羟基的那些,尤其在烷基的β-位(2-位)有羟基的那些。其中取代烷基是支化或未支化的(C2-C6)烷基的(甲基)丙烯酸羟烷基酯单体是优选的。合适的(甲基)丙烯酸羟烷基酯单体包括但不限于:甲基丙烯酸2-羟乙基酯(“HEMA”)、丙烯酸2-羟乙基酯(“HEA”)、甲基丙烯酸2-羟丙酯、甲基丙烯酸1-甲基-2-羟乙基酯、丙烯酸2-羟丙酯、丙烯酸1-甲基-2-羟乙基酯、甲基丙烯酸2-羟丁基酯、丙烯酸2-羟丁基酯和其混合物。优选的(甲基)丙烯酸羟烷基酯单体是HEMA、甲基丙烯酸1-甲基-2-羟乙基酯、甲基丙烯酸2-羟丙酯和其混合物。后两种单体的混合物通常称为“甲基丙烯酸羟丙基酯”或“HPMA”。
可用于本发明的其它取代(甲基)丙烯酸酯和(甲基)丙烯酰胺单体是在烷基中具有二烷氨基或二烷氨基烷基的那些。这种取代(甲基)丙烯酸酯和(甲基)丙烯酰胺单体的例子包括但不限于(甲基)丙烯酸二甲氨基乙基酯(“DMAEMA”)、丙烯酸二甲氨基乙基酯、N,N-二甲氨基乙基甲基丙烯酰胺、N,N-二甲氨基丙基甲基丙烯酰胺、N,N-二甲氨基丁基甲基丙烯酰胺、N,N-二乙氨基乙基甲基丙烯酰胺、N,N-二乙氨基丙基甲基丙烯酰胺、N,N-二乙氨基丁基甲基丙烯酰胺、N-(1,1-二甲基-3-氧代丁基)丙烯酰胺、N-(1,3-二苯基-1-乙基-3-氧代丁基)丙烯酰胺、N-(1-甲基-1-苯基-3-氧代丁基)甲基丙烯酰胺和2-羟乙基丙烯酰胺,氨乙基亚乙基脲的N-甲基丙烯酰胺、N-甲基丙烯酰氧基乙基吗啉、二甲氨基丙基胺的N-马来酰亚胺和其混合物。
可用于本发明的其它取代(甲基)丙烯酸酯单体为含硅单体如(甲基)丙烯酸γ-丙基三(C1-C6)烷氧基甲硅烷基酯、(甲基)丙烯酸γ-丙基三(C1-C6)烷基甲硅烷基酯、(甲基)丙烯酸γ-丙基二(C1-C6)烷氧基(C1-C6)烷基甲硅烷基酯、(甲基)丙烯酸γ-丙基二(C1-C6)烷基(C1-C6)烷氧基甲硅烷基酯、(甲基)丙烯酸乙烯基三(C1-C6)烷氧基甲硅烷基酯、(甲基)丙烯酸乙烯基二(C1-C6)烷氧基(C1-C6)烷基甲硅烷基酯、(甲基)丙烯酸乙烯基(C1-C6)烷氧基二(C1-C6)烷基甲硅烷基酯、(甲基)丙烯酸乙烯基三(C1-C6)烷基甲硅烷基酯和其混合物。
可用作本发明的不饱和单体的乙烯基芳族单体包括但不限于:苯乙烯(“STY”)、α-甲基苯乙烯、乙烯基甲苯、对甲基苯乙烯、乙基乙烯基苯、乙烯基萘、乙烯基二甲苯和其混合物。乙烯基芳族单体还包括其相应的取代对应物,如卤化衍生物,即含一个或多个卤素基团如氟、氯或溴的衍生物;和硝基、氰基、(C1-C10)烷氧基、卤代(C1-C10)烷基、(C1-C10)烷氧羰基、羧基、氨基、(C1-C10)烷基氨基衍生物等。
可用作本发明不饱和单体的含氮化合物和其硫类似物包括但不限于乙烯基吡啶如2-乙烯基吡啶或4-乙烯基吡啶;低级烷基(C1-C8)取代N-乙烯基吡啶如2-甲基-5-乙烯基-吡啶、2-乙基-5-乙烯基吡啶、3-甲基5-乙烯基吡啶、2,3-二甲基-5-乙烯基吡啶和2-甲基-3-乙基-5-乙烯基吡啶,甲基取代的喹啉和异喹啉,N-乙烯基己内酰胺,N-乙烯基丁内酰胺,N-乙烯基吡咯烷酮,乙烯基咪唑,N-乙烯基咔唑,N-乙烯基丁二酰亚胺胺,(甲基)丙烯腈,邻-、间-或对氨基苯乙烯,马来酰亚胺,N-乙烯基噁唑烷酮,N,N-二甲基氨基乙基乙烯基醚,2-氰基丙烯酸乙基酯、乙烯基乙腈,N-乙烯基邻苯二甲酰亚胺,N-乙烯基吡咯烷酮类如N-乙烯基硫吡咯烷酮,3-甲基-1-乙烯基吡咯烷酮、4-甲基-1-乙烯基吡咯烷酮、5-甲基-1-乙烯基吡咯烷酮、3-乙基-1-乙烯基-吡咯烷酮、3-丁基-1-乙烯基吡咯烷酮、3,3-二甲基-1-乙烯基吡咯烷酮、4,5-二甲基-1-乙烯基吡咯烷酮、5,5-二甲基-1-乙烯基吡咯烷酮、3,3,5-三甲基-1-乙烯基吡咯烷酮、4-乙基-1-乙烯基吡咯烷酮、5-甲基-5-乙基-1-乙烯基吡咯烷酮和3,4,5-三甲基-1-乙烯基吡咯烷酮,乙烯基吡咯,乙烯基苯胺和乙烯基哌啶。
可在本发明中用作不饱和单体的取代乙烯单体包括但不限于:烯丙基单体、乙酸乙烯酯、乙烯基甲酰胺、氯乙烯、氟乙烯、溴乙烯、偏二氯乙烯、偏二氟乙烯和偏二溴乙烯。
PNP任选地含有其它官能团,这些官能团通过聚合含这些基团或其前体基团的单体来提供。任选地,通过PNP的离子基团与合适的化合物反应将这些官能团连接于PNP上。例如,通过羧酸基团与合适的醇如封端聚烯化氧反应使含羧酸基团的PNP改性以包含亲水性侧基。或者,官能基团通过非自由基反应而连接于PNP上,由此在含该基团的改性化合物和与PNP共价键合的互补性可反应基团之间形成离子或共价键,如US5,270,380中教导的。
用于本发明的聚合物纳米颗粒可通过乳液聚合、悬浮聚合、非水分散体聚合或溶液聚合制备。这里的“溶液聚合”是指在作为聚合物的溶剂的含水或非水介质中的自由基加成聚合。这里的“聚合物的溶剂”是指不存在交联的聚合物可溶于该聚合介质中,如基于在不存在用于含低于20wt%多烯属不饱和单体的聚合物的交联单体的相同条件下所制备的聚合物的溶解度所预期的,或基于这里公开的溶解度图选取的聚合介质。
聚合物纳米颗粒可在非水溶剂中制备。这些溶剂的例子包括但不限于烃,如链烷烃,氟化烃,和芳烃;醚;酮;酯;醇;和其混合物。特别合适的溶剂包括十二烷、均三甲苯、二甲苯、二苯基醚、γ-丁内酯、乳酸乙酯、丙二醇单甲基醚乙酸酯、己内酯、2-庚酮、甲基异丁基酮、二异丁基酮、丙二醇单甲基醚、癸醇和叔丁醇。
聚合物纳米颗粒可通过首先将溶剂尾料或溶剂和一部分单体的混合物加入装有搅拌器、温度计和回流冷凝器的反应器中来制备。单体投料通常由单体、引发剂和若合适的链转移剂组成。将溶剂或溶剂/单体尾料在搅拌下在氮气氛下加热至约55℃至约125℃的温度。当尾料投料达到足以引发聚合的温度时,将单体投料或余量的单体投料在15分钟至4小时内加入反应器中,同时将反应保持在所需反应温度下。完成单体混合物加料后,可将在溶剂中的另外的引发剂加入反应中和/或采用一段保持时间。
聚合物纳米颗粒可通过乳液聚合制备。通常通过首先将水和单体乳液的一部分加入装有搅拌器、温度计和回流冷凝器的反应器中制备可用于本发明的乳液聚合物。单体乳液通常由单体、表面活性剂、引发剂和若合适的链转移剂组成。将单体乳液的初始投料在搅拌下在氮气氛围中加热至约55℃至约125℃的温度。当种子投料达到足以引发聚合的温度后,将单体乳液或余量的单体乳液在15分钟至4小时内加入反应器中,同时将反应保持在所需反应温度下。完成单体乳液加料后,可将另外的引发剂加入反应中和/或采用一段保持时间。
此外,乳液聚合可在间歇工艺中进行。在这种间歇工艺中,可通过将水、单体、表面活性剂、引发剂和若合适的链转移剂在搅拌下在氮气氛下加入反应容器中制备乳液聚合物。将单体乳液加热至约55℃至约125℃的温度以进行聚合反应。完成单体乳液加料后,可将在溶剂中的另外的引发剂加入反应中和/或采用一段保持时间。
合适的聚合物纳米颗粒包括例如:
HEMA/DEGDMA,MMA/DEGDMA,MMA/MAPS/DEGDMA,MMA/MAPS/PETTA,MMA/MAPS/PPG4000DMA,MMA/MAPS/DPEPA,MAPS/DEGDMA,BA/DEGDMA,MMA/MAPS/TMPTMA,MMA/MAPS/DVB,STY/MAPS/DVB,BA/MAPS/DVB,BA/TMSMA/DVB,BA/MOPTSOMS/DVB,BA/MOPMDMOS/DVB,BA/MAPS/TAT,ALMA/BA/DVB,IBOMA/MAPS/DVB,IBOA/MAPS/DVB,BA/DVB,BA/PGDMA,BA/ALMA,BA/TMPTMA,BA/DPEPA,EHA/DVB,EHA/ALMA,EHA/TMPTMA,EHA/DPEPA,STY/DVB,STY/ALMA,EHA/STY/ALMA,MMA/BA/ALMA,STY/MMA/DVB,MMA/丁二烯/STY,MMA/EA/ALMA,BA/ALMA/MATS,STY/MATS/DVB,MMA/BA/MATS,STY/MMA/MATS/DVB,MMA/BA/MATS/ALMA,BzA/TMPTMA,BzA/DVB,IDMA/BzMA和MMA/ALMA/MATS。
颗粒尺寸和分布的控制可通过例如选择溶剂、选择引发剂、总固含量、引发剂的量和反应条件实现。颗粒尺寸使用标准动态光散射技术测定。所有相关函数用LaPlace转化法如CONTIN转化为流体动力学尺寸。
可用于本发明自由基聚合的引发剂包括例如过氧酯、二烷基过氧化物、烷基氢过氧化物、过硫酸盐、偶氮引发剂、氧化还原引发剂等中的一种或多种。可用的自由基引发剂包括但不限于过氧化苯甲酰、过辛酸叔丁酯、过新戊酸叔戊酯、枯烯氢过氧化物,和偶氮化合物如偶氮异丁腈和2,2′-偶氮双(2-甲基丁腈)。自由基引发剂优选是过新戊酸叔戊酯。自由基引发剂的用量通常为0.05至10wt%,按总单体重量计。
链转移剂任选用于制备可用于本发明的聚合物。合适的链转移剂包括例如:烷基硫醇如十二烷基硫醇;具有活性氢的芳烃如甲苯。
聚合物纳米颗粒还可进行后官能化。这种后官能化可用本领域中已知的任何技术实现。纳米颗粒的后聚合官能化例如对于使颗粒与在塑料组合物中的其它组分相容是有利的。
一个实施方案中,羧酸单体如MAA也存在于纳米颗粒制备中,或若在完成其聚合后将巯基乙酸加成到纳米颗粒中存在的残留双键上,也可赋予填料、颜料和着色剂一定程度的分散性。
按照类似的方式,多烯属不饱和单体可选自DVB、TVB和四甲基丙烯酸季戊四醇酯。若需要确保在纳米颗粒中存在足够量的残余双键,则多烯属不饱和单体的重量分数可增加至50%或更高。这样可允许巯基乙酸或H2S或含PH的化合物随后加成,从而引入以上指出的另外的官能团。的确,当使用高含量的DVB时,可将残余双键环氧化以提供可消除HCl并由此用作PVC的稳定剂的纳米颗粒。
聚合物纳米颗粒有利地是分离的或未聚集的,并可分散、混溶于塑料组合物中或基本上与塑料组合物相容。
所述颗粒与塑料组合物其余组分的相容性一般通过其溶解度参数如VanKrevelen参数δh和δv的匹配性确定。例如,参见,Van Krevelen等人,Properties of Polymer.Their Estimation and Correlation with Chemical Structure,Elsevier Scientific Publishing Co.,1976;Olabisi等人.,Polymer-Polymer Miscibility,Academic Press,NY,1979;Coleman等人.,Specific Interactions and the Miscibility of Polymer Blends,Technomic,1991;and A.F.M.Barton,
CRC Handbook of Solubility Parameters and Other Cohesion Parameters,2nd Ed.,CRC Press,1991.δh是物质的氢键作用参数,δv是物质的分散性和极性相互作用的量度。这种溶解度参数还可通过例如基团贡献法计算,或通过测量由可溶溶剂和不溶溶剂组成的混合溶剂体系中的物质的浑浊点来确定。在浑浊点的溶解度参数定义为溶剂的重量百分比。通常,测量物质的多个浑浊点,并且将这些浑浊点定义的中心区域定义为物质的溶解度参数区域。
当颗粒和塑料的溶解度参数基本上类似时,该颗粒与塑料相容,并且不太可能出现相分离和/或颗粒的聚集。优选颗粒和塑料的溶解度参数,尤其δh和δv,基本上匹配。
聚合物纳米颗粒可以以在聚合溶剂中的分散体的形式使用,或它们可通过例如真空蒸发、通过沉淀入非溶剂中和喷雾干燥分离;该分离的纳米颗粒可随后再分散于适于加入塑料中的介质中。
可以如本领域技术人员公知的那样,通过将颗粒或颗粒的分散体与其它溶解的或分散的聚合物和/或其它塑料助剂掺混,将聚合物纳米颗粒引入塑料中。塑料组合物中的另外的组分如UV稳定剂、颜料、PVC树脂、消光剂、流动助剂、加工助剂、润滑剂、填料、稳定剂等可以粉末或液体形式与树脂粉末掺混。可将各种添加剂例如UV稳定剂乳化、加入塑料聚合物分散体中并共喷雾干燥。或者,乳化的添加剂,如颜料分散体可在合适的允许加热和除去水的混合器中直接加入树脂粉末中。此外,PVC湿饼可与粉末或水基纳米颗粒分散体混合。混合乳液基添加剂和粉末接着干燥的各种组合是本领域技术人员能够想到的。
在一个实施方案中,可在塑料合成之前、过程中或之后,将纳米颗粒加工助剂加入用于制备塑料如PVC的悬浮液、溶液、气相喷雾或乳液体系中。纳米颗粒可迁移到这些颗粒材料的表面并被带入到配混操作中。纳米颗粒可与其它改性剂如冲击改性剂一起加入。纳米颗粒组合物还可包括赋予润滑性的共聚单体如甲基丙烯酸正十二烷基酯和正十八烷基酯,这样同时赋予共混物以加工助剂和固有润滑性能。
在另一实施方案中,粒料形式的聚合物纳米颗粒是可以想到的。这些粒料一般用于制备热塑性塑料薄膜、片材和其它各种制品。为避免粉末常遇到的一些问题,如形成灰尘,粒料形式通常比使用粉末形式更合适。因此,粉末可用任何合适的塑料造粒装置和塑料加工领域已知的其它各种方法形成粒料。这些粒料形成步骤可与混合步骤结合其中塑料组合物的组分可使用标准塑料加工装置配混(混合)并造粒。
在本发明的一个实施方案中,将具有1至100纳米直径的聚合物纳米颗粒以2-30pphr的量加入热塑性树脂,优选PVC中,从而相对于具有常规冲击改性剂的相同PVC组合物,提供改进的冲击强度和改进的光学透明性。具有<25℃的玻璃化转变温度的纳米颗粒,特别是粒径低于20nm的(甲基)丙烯酸均聚或共聚物,丁二烯与其它乙烯基单体的共聚物,或弹性体组合物如腈类橡胶、EPDM和EVA是优选的。
本发明的一个实施方案中,具有1至100nm直径的聚合物纳米颗粒加入聚碳酸酯树脂组合物中。优选使用0.5至20wt%,更优选0.5至5wt%的纳米颗粒,按所用树脂计。优选选择纳米颗粒组合物,如MMA为主要量的(MMA/BA/TMPTMA)。与无纳米颗粒的相同组合物相比,聚碳酸酯塑料组合物显示改进的冲击强度,同时保持了碳酸酯的透明度。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒加入尼龙组合物、聚(对苯二甲酸丁二醇酯)组合物、聚(对苯二甲酸乙二醇酯)组合物或上述组合物相互或与其它工程塑料如聚碳酸酯的共混物中。优选使用0.5至20wt%,更优选0.5至5wt%的纳米颗粒,基于所用树脂。优选选取纳米颗粒组合物如(MMA/BA/羧酸单体/TMPTMA),(MMA/BA/GMA/TMPTMA),(MMA/BA/马来酸酐/TMPTMA),(MMA/BA/DMAEMA/TMPTMA),(STY/羧酸单体/DVB),(STY/GMA/DVB),(STY/马来酸酐/DVB),(STY/HEMA/DVB),或(STY/DMAEMA/DVB)。最终组合物显示增强的熔体强度,因此可用于生产通过要求熔体强度的各种加工路线制备的制品,其中包括来自管吹膜法的薄膜、热成型部件、注坯吹塑瓶等。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒和更大的聚合物颗粒引入到塑性树脂,优选PVC中,最终的颗粒共混物是本领域技术人员称为双模态冲击改性剂的冲击改性组合物。优选使用0.5至20wt%的颗粒(按树脂计),其中10至90wt%的颗粒为具有1至100nm直径的聚合物纳米颗粒。优选选取纳米颗粒组合物,如主要量为MMA的(MMA/BA/TMPTMA)、EGMA/TMPTMA或PPGMA/TMPTMA。尽管不受机理束缚,但据信纳米颗粒在某些塑料中会引起剪切屈服/微裂纹,其中第二个、更大的方式可按龟裂停止方式发挥作用或作为剪切屈服增强剂(若其空穴化)。双模态冲击改性剂塑料组合物相对于无纳米颗粒的相同组合物显示改进的冲击强度。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒以0.1至15pphr、优选0.1至2pphr、更优选0.1至1%pphr加入到热塑性树脂、优选PVC中,以提供在树脂的熔体流变性能上的改进,从而用作在本领域中称为加工助剂的组合物。在组成上包括(甲基)丙烯酸系共聚物,任选有其它乙烯基单体,优选含有大于70wt%MMA并且重均分子量大于500,000的那些共聚物的纳米颗粒是优选的。该改性树脂组合物提供改进的清澈透明的挤出和注塑产品。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒以2至30pphr的量加入到热固性树脂,优选液体基环氧化物或不饱和聚酯中,以提供在冲击强度上的改进和在总组合物的粘度上的最小增加。颗粒直径为1至50nm、优选1至20nm的纳米颗粒可用于其中需要光学透明性的透明凝胶涂料中和用于含增强纤维的增强热固性复合材料中。
在本发明的一个实施方案,将具有1至100nm直径的聚合物纳米颗粒以2-30pphr的量加入到热固性树脂中,以提供在固化树脂的低收缩和表面光滑度方面的改进,即用作低表面粗糙度添加剂,而在总组合物的粘度上的提高最小。相对于使用更大颗粒尺寸聚合物低表面粗糙度添加剂,可注意到改进。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒以2至30phr的量加入到热塑性树脂如PVC中,以降低它的热膨胀系数而不改变树脂的其它重要性能。调节树脂的热膨胀系数不仅对于在冷却熔体时控制其固有收缩趋势是重要的,而且在该树脂与其它树脂共挤出或层压时,控制各热膨胀系数的能力可导致通过那些方式生产的产品的所需性能和最终形式。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒以2至50phr的量加入到热塑性树脂如PVC中,以提高其耐热变形温度(HDT)。这在诸如壁板(siding)、热水管和装配件(fitting)之类的应用中是重要的。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒以2至30pphr的量加入到热固性树脂中,提供在树脂的颜料着色性能上的改进。相对于更大颗粒尺寸的聚合物添加剂如目前使用的苯乙烯、聚乙酸乙烯酯、丙烯酸树脂和聚酯,可以看出有改进。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒加入到塑料树脂组合物,优选聚烯烃中,起到成核剂的作用。优选使用基于树脂的0.01至2wt%的纳米颗粒。优选选取引入了与苯乙烯、4-甲基苯乙烯、(甲基)丙烯酸异冰片酯、氟化单体如ZONYLTM单体或氟化乙烯衍生物、支链烷烃羧酸(versatic acid)不饱和衍生物如VEOVATM单体,或(甲基)丙烯酸“中级”或“高级”烷基酯共聚合的多官能单体的纳米颗粒组合物。该塑料组合物相对于无纳米颗粒的相同组合物显示更高的结晶度。
在本发明的一个实施方案中,将具有互补官能团的官能化聚合物纳米颗粒加入塑料树脂组合物中,所述互补官能团能够相互作用如相互进行离子或共价反应,纳米颗粒具有1至100nm的直径。优选使用基于树脂的1至20wt%的纳米颗粒。选择可分散在树脂中但具有官能团的官能化纳米颗粒,该官能团可相互反应形成颗粒的链以进行自组装。这可通过将具有官能团“A”(胺,酸)的纳米颗粒与具有互补官能团“B”(环氧、酸酐)的纳米颗粒混合来实现。纳米颗粒的本体除了包括多烯属不饱和单体外还包括促进在给定的塑料树脂中的分散性的单体(例如用于聚烯烃的LMA或SMA),但是低含量的官能团(优选位于颗粒的外层中)将促进颗粒间的相互作用。或者,合适的低分子量官能化合物或官能化聚合物可用作组装促进剂,即促进(大)网络形成。与无纳米颗粒的相同组合物相比,该塑料组合物显示改进的流变控制,和/或增强和/或改进的输运性能。
在本发明的一个实施方案中,将具有1至100nm直径的聚合物纳米颗粒加入塑料树脂如聚碳酸酯和尼龙中。优选使用0.5至20wt%,更优选0.5至5wt%(基于树脂)的纳米颗粒。优选选取纳米颗粒组合物,如主要量为MMA的(MMA/BA/TMPTMA)。这些颗粒包括用于在聚合物破碎(聚合物结构的疲劳)时进行龟裂愈合(crack healing)的液体状或低聚物质,如Nature,Vol.409,794(2001)中公开的。
给出下面的实施例进一步说明本发明的各个方面。
实施例1.制备聚合物纳米颗粒
将500mL反应器装上热电偶、温度控制器、吹扫气体入口、带有吹扫气体出口的水冷却回流冷凝器、搅拌器和加料漏斗。向加料漏斗中投入201.60g由18.00g甲基丙烯酸甲酯(纯度100%)、2.00g二甲基丙烯酸二甘醇酯(纯度100%)、1.60g过氧新戊酸叔戊基酯在矿物油精中的75%溶液(Luperox554-M-75)和180.00g二异丁基酮(“DIBK”)组成的单体混合物。然后将含180.00g DIBK的反应器用氮气吹扫30分钟,接着将反应器中的物料加热至75℃。当反应器中的物料达到75℃时,将加料漏斗中的单体混合物在90分钟内均匀投入反应器中。在单体混合物加料结束后的30分钟,添加间隔30分钟并由0.06g的过氧新戊酸叔戊基酯在矿物油精中的75%溶液(Luperox 554-M-75)和2.00g DIBK组成的两个追加等分试样当中的第一个。在第二个追加等分试样的添加结束后,将反应器中的物料在80℃下保持2.5小时以完成反应。将所得聚合物通过用庚烷沉淀进行分离,过滤收集并在真空下干燥,得到白色粉末。将此物料重新溶于丙二醇单甲基醚乙酸酯中。如此形成的纳米颗粒的颗粒尺寸分布为0.8至5.0nm,平均尺寸为1.4nm(通过动态激光散射法测定),分子量约22,642g/mol,数均分子量约14,601g/mol,Mw/Mn分布为1.6(通过GPC测定)。
实施例2.制备聚合物纳米颗粒:
通过半间歇乳液聚合法制备AAEM/ALMA共聚物。
由17g去离子水、8.85g 28%w/w固体的月桂基硫酸铵(“ALS”)、12.4g甲基丙烯酸乙酰乙酰氧基乙酯(“AAEM”)和1.78g甲基丙烯酸烯丙基酯(”ALMA”)的混合物制备单体乳液。由600g去离子水、15.0g 28%w/w固体的ALS和在1mL去离子水中的0.15g过硫酸铵(“APS”)制备反应釜料。将反应釜料在用氮气吹扫下加热至90℃。将一半单体乳液在以200rpm搅拌下加入反应釜料中。20分钟后,加入剩余单体乳液。将釜温在90℃下保持30分钟、冷却至55℃,然后分别加入0.02g叔丁基过氧化氢(“t-BHP”)在1mL去离子水中的溶液和0.010g甲醛次硫酸钠(“SSF”)在1mL去离子水中的溶液。将反应冷却至环境温度并将乳液分别通过400和100目筛子过滤。
将样品通过冷冻干燥从水中分离,由此生产白色易碎的自由流动粉末。将所得白色粉末用大量的二次蒸馏和去离子的水洗涤以除去大部分表面活性剂。
实施例3.制备聚合物纳米颗粒:
通过间歇乳液聚合法制备AAEM/ALMA共聚物。
由17g去离子水、8.85g 28%w/w固体的ALS、12.4g AAEM和1.78g ALMA的混合物在瓶中制备单体乳液。由600g去离子水、15.0g 28%w/w固体的ALS和在1mL去离子水中的0.15g APS制备反应釜料。将反应釜料在用氮气吹扫下加热至90℃。将单体乳液在以200rpm搅拌下一次全部加入反应釜料中。30分钟后,反应烧瓶温度冷却至75℃,然后加入0.02g t-BHP在1mL去离子水中的溶液。将反应进一步冷却至55℃,并加入0.010g SSF在2mL去离子水中的溶液。将反应冷却至环境温度并将乳液分别通过400和100目筛子过滤。
实施例4.通过逐步加成聚合法制备聚合物纳米颗粒。
由100g水、1.60g 28%w/w固体的ALS、68g丙烯酸乙酯(“EA”)、17g甲基丙烯酸甲酯(“MMA”)、12.5g二乙烯基苯(“DVB”)和5g甲基丙烯酸(“MAA”)的混合物制备单体乳液。将包含445g水、22.2g 28%w/w固体的ALS和0.37g APS的反应釜料在氮气氛下加热至85℃。将单体乳液在90分钟内加入反应釜中。加料结束后将反应在85℃保持30分钟,然后冷却至65℃。冷却后,加入1.33g 10%硫酸亚铁(FeSO4)。1分钟后,加入0.2g 70%的t-BHP,2分钟后加入0.10g 100%异抗坏血酸(“IAA”)并将反应保持15分钟。按相同的顺序并在相同的时间间隔内加入第二追加料体系。将反应冷却至环境温度并通过400目筛子过滤。
实施例5:制备各种聚合物纳米颗粒
聚合物的纳米颗粒组成记载在表5.1中。这些聚合物按照实施例1-4的通用程序制备。简写“Mw”指重均分子量,术语“Mn”指数均分子量。简写“Dist”指Mw/Mn。分子量用标准GPC法(用四氢呋喃作为溶剂)测量。
表5.1:聚合物纳米颗粒组成
样品5- 组成 比率 Mw Mn Dist
1 HEMA/DEGDMA 90/10
2 MMA/DEGDMA 90/10
3 MMA/DEGDMA 90/10 19073 11183 1.7
4 MMA/DEGDMA 90/10 644 221 2.9
5 MMA/DEGDMA 90/10 771 3989 1.9
6 MMA/MAPS/DEGDMA 70/20/10 10640 4254 2.5
7 MMA/MAPS/DEGDMA 80/10/10 12819 8091 1.6
8 MMA/MAPS/DEGDMA 60/30/10
9 MMA/MAPS/DEGDMA 40/50/10 43667 9047 4.8
10 MMA/MAPS/DEGDMA 20/70/10 166432 7404 22.5
11 MAPS/DEGDMA 90/10 11683 3484 3.4
12 MMA/MAPS 88.9/11.1 15965 7424 2.2
13 BA/DEGDMA 90/10 51007 29065 1.8
14 MMA/MAPS/PETTA 80/10/10
15 MMA/MAPS/ 80/10/10
PPG4000DMA
16 MMA/MAPS/DPEPA 80/10/10
17 MMA/MAPS/TMPTMA 80/10/10
18 MMA/MAPS/DEGDMA 75/10/15
19 MMA/MAPS/DEGDMA 85/10/5
20 MMA/MAPS/DVB 10/60/30 95613 12003 8.0
21 MMA/MAPS/DVB 20/60/20 110422 19814 5.6
22 MMA/MAPS/DVB 25/60/15
23 MMA/MAPS/DVB 30/60/10
24 MMA/MAPS/DEGDMA 20/70/10 35249 7438 4.7
25 MMA/MAPS/DEGDMA 30/60/10 35105 7003 5.3
26 MMA/MAPS/DVB 10/80/10 331732 29918 11.1
27 STY/MAPS/DVB 30/60/10 38455 12320 3.1
28 BA/MAPS/DVB 30/60/10 499094 36317 13.7
29 BA/MAPS/DVB 10/80/10 312848 16102 19.4
30 BA/TMSMA/DVB 10/80/10 674730 30989 21.8
31 BA/MOPTSOMS/DVB 10/80/10 97530 12154 8.0
32 BA/MOPMDMOS/DVB 10/80/10 363561 37553 9.7
33 BA/MAPS/TAT 10/80/10 12201 5182 2.4
34 ALMA/BA/DVB 10/80/10
35 IBOMA/MAPS/DVB 10/80/10
36 BA/DVB 90/10 223436 29309 7.6
37 BA/PGDMA 90/10 26797 8242 3.3
38 BA/ALMA 90/10 104529 15967 6.5
39 BA/TMPTMA 90/10 39638 16306 2.4
40 BA/DPEPA 90/10 103945 18702 5.6
41 EHA/DVB 90/10
42 EHA/ALMA 90/10
43 EHA/TMPTMA 90/10
44 EHA/DPEPA 90/10
45 STY/DVB 90/10
46 STY/ALMA 90/10
47 EHA/STY/ALMA 20/70/10
48 EHA/STY/ALMA 45/45/10
49 MMA/DEGDMA 90/10 22642 14601 1.6
实施例6.制备含纳米颗粒加工助剂的PVC组合物。
将与过氧新戊酸叔戊基酯(0.5份)混合的MMA(90份)和TMPTMA(10份)在1小时内加入到回流着的MIBK(200份)中。继续加热1小时以提供加工助剂的“溶液”。可将纳米颗粒分离并加入PVC树脂中,由此提供相对于单独PVC的流变性能而言改进的加工流变性能。
Claims (4)
1.一种塑料组合物,包括具有1至100nm直径的聚合物纳米颗粒和塑料组分,其中所述塑料组分包括下列材料中的至少一种:尼龙组合物、聚(对苯二甲酸丁二醇酯)组合物、聚(对苯二甲酸乙二醇酯)组合物或上述组合物与其它工程塑料如聚碳酸酯组合物的共混物。
2.一种塑料组合物,包括具有1至100nm直径的聚合物纳米颗粒和塑料组分,其中所述塑料组分包括PVC,并且其中所述纳米颗粒以每100份所述塑料组分2至50份的浓度存在于塑料组合物中。
3.如权利要求2的塑料组合物,其中所述纳米颗粒以每100份所述塑料组分2至30份的浓度存在于塑料组合物中。
4.一种提供塑料组合物的方法,包括:
a.形成具有1至100nm直径的聚合物纳米颗粒;和
b.获得包括至少一种如下材料的塑料组分:尼龙组合物、聚(对苯二甲酸丁二醇酯)组合物、聚(对苯二甲酸乙二醇酯)组合物或上述组合物与其它工程塑料如聚碳酸酯组合物的共混物;和
c.形成包括所述聚合物纳米颗粒和所述塑料组分的塑料组合物。
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US9416300B2 (en) | 2011-01-16 | 2016-08-16 | Simpson Strong-Tie Company, Inc. | Low temperature curable adhesive compositions |
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CN103608415A (zh) * | 2011-01-16 | 2014-02-26 | 辛普森强力连接公司 | 低温可固化粘合剂组合物 |
US9416300B2 (en) | 2011-01-16 | 2016-08-16 | Simpson Strong-Tie Company, Inc. | Low temperature curable adhesive compositions |
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