CN114058009B - 减少二胺单体损失的半芳族聚酰胺制备方法及半芳族聚酰胺和模塑组合物 - Google Patents
减少二胺单体损失的半芳族聚酰胺制备方法及半芳族聚酰胺和模塑组合物 Download PDFInfo
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- CN114058009B CN114058009B CN202111519562.3A CN202111519562A CN114058009B CN 114058009 B CN114058009 B CN 114058009B CN 202111519562 A CN202111519562 A CN 202111519562A CN 114058009 B CN114058009 B CN 114058009B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明属于聚酰胺技术领域,具体涉及一种减少二胺单体损失的半芳族聚酰胺制备方法及半芳族聚酰胺和模塑组合物。所述的减少二胺单体损失的半芳族聚酰胺制备方法,包括以下步骤:(1)以二元羧酸单体A和二元胺单体B为原料,在催化剂和封端剂的作用下,在水中进行聚合反应2~12h后,再加入高沸点二胺单体C和/或低分子量富胺齐聚物D,继续聚合反应,得到预聚物;(2)将预聚物进行固相增粘或熔融缩聚反应,得到半芳族聚酰胺。本发明在聚合初期保证二酸单体过量,聚合后期通过补加高沸点二胺单体或富胺齐聚物,减少了聚合过程排气阶段二胺单体的损失,具有良好的经济价值和环保价值。
Description
技术领域
本发明属于聚酰胺技术领域,具体涉及一种减少二胺单体损失的半芳族聚酰胺制备方法及半芳族聚酰胺和模塑组合物。
背景技术
聚酰胺是指主链含有酰胺键(-CONH-)的一类聚合物。由于酰胺键的存在,聚酰胺分子链间存在较强的氢键作用,氢键的存在促进了聚酰胺树脂的结晶,同时增强了聚酰胺分子链间的相互作用,因而聚酰胺树脂具有良好的力学性能、耐磨性能、耐化性能等。聚酰胺树脂通常以管材、型材、制件、薄膜或纤维等形式应用于多种领域,例如汽车、电子电器、建筑建材、照明、航空航天领域等。
由于半芳族聚酰胺具有更高的熔点,通常大于300℃,因此半芳族聚酰胺一般无法通过类似PA66或PA6的聚合工艺来合成。传统的半芳族聚酰胺一般先采用溶液成盐缩聚工艺,在高温高压条件下预聚,通过水的逐步排除,促使聚合反应向生成高分子量方向进行。待聚合度达到一定程度,获得预聚物,预聚物通过进一步固相聚合或熔融聚合得到高分子量的半芳族聚酰胺树脂。依据后缩聚的实施方式不同,一般将半芳族聚酰胺的合成工艺分为固相聚合工艺和熔融缩聚工艺。
在聚合过程中,为保证聚合反应的顺利进行,需将聚合体系中的水逐步排出至反应体系外。由于二胺单体具有较高的挥发性,在体系排水过程中,不可避免的导致少量的二胺单体跟随水汽一同排出至聚合体系外。少量二胺单体的排出导致聚合体系中的物料失衡,对缩聚反应而言,物料单体的配比失衡将导致聚合后期无法获得高分子量的聚合物,影响最终的产品性能。工业上,常见的解决办法为采用高温高压聚合工艺,同时将二胺单体的加入量保持稍过量来弥补二胺单体的损失。然而,二胺单体的过量导致过量部分二胺单体无法与二酸单体成盐,游离状态的二胺单体更容易挥发,在聚合过程中损失。此外,由于聚合过程中排出水汽中含有少量的二胺单体,从而产生大量含有二胺单体的废水,从经济角度和环保角度来讲,均不利于生产的扩大和运营。
发明内容
本发明要解决的技术问题是:提供一种减少二胺单体损失的半芳族聚酰胺制备方法,大大降低了聚合过程中二胺单体的损失,具有良好的经济价值和环保价值;本发明还提供制备的半芳族聚酰胺和其组成的模塑组合物。
第一方面:
本发明所述的减少二胺单体损失的半芳族聚酰胺制备方法,包括以下步骤:
(1)以二元羧酸单体A和二元胺单体B为原料,在催化剂和封端剂的作用下,在水中进行聚合反应2~12h后,再加入高沸点二胺单体C和/或低分子量富胺齐聚物D,继续聚合反应,得到预聚物;
(2)将预聚物进行固相增粘或熔融缩聚反应,得到半芳族聚酰胺。
本发明中,所述二元羧酸单体A为含有4~36个碳原子的二元羧酸单体,包括脂肪结构二羧酸单体、脂环结构二羧酸单体和/或芳香结构二羧酸单体,脂肪结构或脂环结构二元羧酸单体。诸如丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一烷二羧酸、十二烷二羧酸、十三烷二羧酸、十四烷二羧酸、十五烷二羧酸、十六烷二羧酸、十七烷二羧酸、十八烷二羧酸、十九烷二羧酸、二十烷二羧酸、2-甲基己二酸、2,2-二甲基戊二酸、3,3-二乙基丁二酸、马来酸、富马酸、衣康酸、二聚体酸、顺式和/或反式环己烷-1,2-二羧酸、顺式和/或反式环己烷-1,3-二羧酸、顺式和/或反式环己烷-1,4-二羧酸、顺式和/或反式环戊烷-1,2- 二羧酸、顺式和/或反式环戊烷-1,3-二羧酸、2-甲基戊二酸中的一种或多种;芳香结构二羧酸单体诸如对苯二甲酸、间苯二甲酸、邻苯二甲酸、2,6-奈二甲酸、2,7-奈二甲酸、1,4-奈二甲酸、1,4-亚苯基二氧基二乙酸、1,3-亚苯基二氧基二乙酸、2,2’-联苯二甲酸、4,4’-氧化双(苯甲酸)、二苯基甲烷-4,4’-二羧酸、二苯基砜-4,4’-二羧酸、4,4’-联苯二羧酸、呋喃二甲酸及其组合。
本发明中,所述二元胺单体B为含有2~36个碳原子的二元胺单体,包括脂肪结构二元胺单体、脂环结构二元胺单体和/或芳香结构二元胺单体,脂肪结构或脂环结构二元胺单体。诸如乙二胺、1,4-丁二胺、1,5-戊二胺、1,6-己二胺、1,7-庚二胺、1,8-辛二胺、1,9-壬二胺、1,10- 癸二胺、1,11-十一碳二胺、1,12-十二碳二胺、1,13-十三碳二胺、1,14-十四碳二胺、1,15-十五碳二胺、1,16-十六碳二胺、1,17-十七碳二胺、1,18-十八碳二胺、1,19-十九碳二胺、1,20-二十碳二胺、2-甲基-1,5-戊二胺、3-甲基-1,5-戊二胺、2-丁基-2-乙基-1,5-戊二胺、2,4-二甲基-1,6- 己二胺、2,2,4-三甲基-1,6-己二胺、2,4,4-三甲基-1,6-己二胺、2-甲基-1,8-辛二胺、5-甲基-1,9- 壬二胺、2,4-二甲基-辛二胺、1,3-双(端胺基甲基)环己烷、双(4-氨基环己基)甲烷、3,3’-二甲基 -4,4’-二氨基二环己基甲烷、异氟尔酮二胺、降莰烷二甲胺、顺-1,4-环己烷二胺、反-1,4-环己烷二胺、甲基环己烷二胺、双(氨丙基)哌嗪、氨乙基哌嗪中的一种或多种;芳香结构二元胺单体诸如间苯二甲胺、对苯二甲胺、对苯二胺、间苯二胺、双(4-氨基苯基)甲烷、3-甲基联苯胺、2,2-双(4-氨基苯基)丙烷、1,1-双(4-氨基苯基)环己烷、1,4-二氨基萘、1,5-二氨基萘、2,6- 二氨基萘、1,3-二氨基甲苯、N,N’-二甲基-4,4’-联苯二胺、双(4-甲基氨基苯基)甲烷、2,2-双(4- 甲基氨基苯基)丙烷中的一种或多种。
二元羧酸单体A的摩尔总数为a,二元胺单体B摩尔总数为b,并且满足a>b。其中当二元羧酸单体A为单一化合物时,摩尔总数a为单一化合物的摩尔数。当二元羧酸单体A为多种二元羧酸单体的混合物时,摩尔总数a为多种二元羧酸单体混合物的摩尔数之和。对于二元胺单体B同理。二元羧酸单体A和二元胺单体B的摩尔比r=a/b,其中r的取值范围为 1~2,优选r在1.01~1.5之间。
本发明中,所述高沸点二胺单体C为在标准大气压下沸点大于220℃的二胺化合物,包括1,8-辛二胺、1,9-壬二胺、1,10-癸二胺、1,11-十一碳二胺、1,12-十二碳二胺、1,13-十三碳二胺、1,14-十四碳二胺、1,15-十五碳二胺、1,16-十六碳二胺、2-甲基-1,8-辛二胺、5-甲基-1,9- 壬二胺、2,4-二甲基-辛二胺、双(4-氨基环己基)甲烷、3,3-二甲基-4,4-二氨基二环己基甲烷、 N’-(6-氨基已基)-己烷-1,6-二胺、N’-(12-氨基十二烷基)十二烷-1,12-二胺、N’-(6-氨基已基) 二烷-1,12-二胺、N’-[3-(氨基甲基)-3,5,5-三甲基环已基]已烷-1,6-二胺、N’-[3-(氨基甲基)-3,5,5- 三甲基环己基]十二烷-1,12-二胺、N’-[(5-氨基-1,3,3-三甲基环己基)甲基]己烷-1,6-二胺、N’-[(5- 氨基-1,3,3-三甲基环己基)甲基]十二烷-1,12-二胺、3-[[[3-(氨基甲基)-3,5,5-三甲基环已基]氨基]甲基]-3,5,5-三甲基环胺、3-[[(5-氨基-1,3,3-三甲基环已基)甲基氨基]甲基]-3,5,5-三甲基环已胺、 3-(氨基甲基)-N-[3-(氨基乙基)-3,5,5-三甲基环己]-3,5,5-三甲基环胺、异氟尔酮二胺、甲基环己烷二胺、间苯二甲胺、对苯二甲胺及其组合。
本发明中,所述低分子量富胺齐聚物D为上述二元羧酸单体A和二元胺单体B反应所得端胺基含量大于端羧基含量的低分子量聚合物,其分子量范围为100~5000g/mol,更优选 150~3000g/mol。端胺基含量和端羧基含量可以通过滴定方法测得。
二元羧酸单体A的摩尔总数为a,二元胺单体B摩尔总数为b,高沸点二胺单体C和/或低分子量富胺齐聚物D的摩尔总数为c,定义参数R=a/(b+c),其中R的取值范围为0.85~1.2。
高沸点二胺单体C和/或低分子量富胺齐聚物D在聚合反应后期加入,随聚合反应进行到后期,反应体系中排出大部分水后,再通过加料装置加入高沸点二胺单体C和/或低分子量富胺齐聚物D来补齐物料配比,得到预聚物;所得预聚物通过固相增粘或熔融缩聚反应即可得到高分子量半芳族聚酰胺。由于在主要排气过程中,二酸单体摩尔数过量,聚合体系中游离状态的二胺单体浓度低,大大降低了聚合过程中二胺单体的损失。
本发明中,另一种实施方案为高沸点二胺单体C和/或分子量富胺齐聚物D可以在熔融缩聚过程中加入,通过挤出机的侧喂料或与预聚物混合后通过挤出机主喂料加入,在熔融聚合过程中达到一定物料配比,得到高分子量的半芳族聚酰胺,其中半芳族聚酰胺的数均分子量优选大于5000g/mol,更优选大于10000g/mol。
本发明中,在步骤(1)聚合反应开始时还可以加入内酰胺和/或氨基酸,所述内酰胺和/ 或氨基酸选择丙-3-内酰胺(β-内酰胺;β-丙内酰胺)、丁-4-内酰胺(γ-内酰胺;γ-丁内酰胺)、2-哌啶酮(δ-内酰胺;δ-戊内酰胺)、己内酰胺(ε-内酰胺;ε-己内酰胺)、α,ω-氨基己酸、庚-7-内酰胺(ζ-内酰胺;ζ-庚内酰胺)、α,ω-氨基壬酸、壬-9-内酰胺(θ-内酰胺;θ-壬内酰胺)、癸 -10-内酰胺(ω-癸内酰胺)、α,ω-氨基十一酸、月桂内酰胺、ω-氨基十二酸、η-辛内酰胺(η-内酰胺;η-辛内酰胺)或其组合,内酰胺和/或氨基酸的加入量为聚合单体摩尔总数的的0~90%。
本发明中,合适的催化剂选自无机和/或有机磷、锡或铅化合物及其混合物。
作为合适的含磷化合物有磷酸、亚磷酸、次磷酸、苯基磷酸、苯基次磷酸和/或与其单价或三价阳离子的盐,和/或其酯,例如磷酸三苯酯、亚磷酸三苯酯或亚磷酸三(壬基苯基)酯。
作为合适的锡类催化剂有氧化锡、氢氧化锡、单羧酸或多羧酸的锡盐。诸如二苯甲酸锡、二(2-乙基己酸)锡、草酸锡、氧化二丁基锡、丁基锡酸、二月硅酸锡等。
作为合适的铅化合物有氧化铅、氢氧化铅、乙酸铅、碱式乙酸铅、碳酸铅等。
特别优选的催化剂为次磷酸及其盐,如次磷酸钠或钾。
催化剂的用量为聚合单体总重量的0.0001~5wt%,优选为10~1000ppm,最优选为 100~500ppm。
本发明中,合适的封端剂选自脂肪结构单羧酸化合物、脂环结构单羧酸化合物、芳香结构单羧酸化合物、脂肪结构单胺化合物、脂环结构单胺化合物和芳族单胺化合物中的一种或多种。
上述单羧酸包括乙酸、丙酸、正丁酸、异丁酸、叔丁酸、戊酸、新戊酸、二甲基乙酸、己酸、庚酸、辛酸、壬酸、癸酸、十一烷酸、月桂酸、十三烷酸、肉豆蔻酸、棕榈酸、硬脂酸、环丙烷羧酸、环戊烷羧酸、环戊烷乙酸、环己烷羧酸、苯甲酸、对甲基苯甲酸、邻甲基苯甲酸、间甲基苯甲酸、对叔丁基苯甲酸、水杨酸、对甲氧基苯甲酸、α-萘甲酸、β-萘甲酸、甲基萘羧酸、苯乙酸、油酸、乳酸、蓖麻油酸、亚油酸、亚麻酸、芥酸、及来自植物的各种脂肪酸,丙烯酸、甲基丙烯酸及以上化合物的混合物。
上述单胺化合物包括甲胺、乙胺、丙胺、丁胺、戊胺、己胺、庚胺、辛胺、癸胺、十八烷胺、二甲胺、二乙胺、二丙胺、二丁胺、环己胺、二环己胺、苯胺、甲苯胺、二苯胺、萘胺、及其混合物。
特别优选的封端剂为乙酸、丙酸、苯甲酸中的至少一种。
封端剂的用量为聚合单体总重量的0.01~10wt%,优选为0.1~5wt%,最优选为0.2~0.8 wt%。
本发明中,聚合反应的反应温度为200-300℃,反应压力为0.5-5MPa。聚合反应是指将二元羧酸单体A与二元胺单体B形成的尼龙盐、内酰胺和/或氨基酸、去离子水、催化剂和封端剂在200-300℃温度下,0.5-5MPa的压力下,通过不断将反应容器中水汽释放,将反应向聚合反应方向推进,得到具有一定分子量的半芳族聚酰胺齐聚物。
聚合反应过程中,当聚合体系中通过排气,排出体系中大部分水后,残余水质量含量为 1-35%,通过加料装置向聚合体系中补加高沸点二胺单体C和/或分子量富胺齐聚物D,继续聚合反应得到预聚物。
本发明中,固相增粘反应在惰性气体氛围或真空条件下进行,反应温度220-280℃,反应时间2-24小时;熔融缩聚在带有排气口的挤出设备中进行,反应温度280-350℃,反应时间在0.5小时以内。
第二方面:
本发明所述的半芳族聚酰胺,由上述制备方法制备得到,其熔点为250-350℃,熔点通过差式扫描量热法(DSC)测定。
第三方面:
本发明所述的半芳族聚酰胺组成的模塑组合物,包括以下重量份数的原料:
其中,增强材料选自玻璃纤维、钛酸钾纤维、钛酸钾晶须、金属包层的玻璃纤维、碳纤维、陶瓷纤维、硅灰石纤维、莫来石纤维、二氧化硅纤维、石英纤维、陶瓷纤维、玄武岩纤维、金属纤维、金属碳化物纤维、金属固化纤维、石棉纤维、氧化铝纤维、碳化硅纤维、硼纤维、碳酸钙晶须、硼酸铝晶须、氧化锌晶须、芳纶纤维、液晶聚酯纤维、尼龙纤维、超高分子量聚乙烯纤维、聚酰亚胺纤维、聚苯硫醚纤维、聚苯并咪唑纤维、聚苯并恶唑纤维、聚芳醚酮纤维、木纤维、亚麻纤维、大麻纤维和剑麻纤维、天然纤维中的一种及其组合。优选为玻璃纤维、碳纤维、芳纶纤维、硼纤维、金属纤维、钛酸钾纤维中的至少一种。
无机类填料包括纤维状、颗粒状、纳米颗粒形态填料,如玻璃微珠、陶瓷微珠、高岭土、白垩、粘土、铝硅土、硫化锌、硫化锶、硫化钡、钛酸铅、钛酸钡、二硫化钼、聚四氟乙烯、二氧化钛、二氧化硅、碳酸钡、碳酸镁、氮化铝、氮化硼、碳化硅、钛酸钾、钛酸钾晶须、硼酸锌、磷酸锌、磷酸钙、硼酸铝、硼酸铝晶须、炭黑、石墨、石墨烯、碳纳米管、纳米氧化铝、硅酸盐、硅酸铝、硅酸钙、硅酸镁、碱式硅酸锌、氧化钙、氧化镁、氧化锆、氧化钛、氧化铁、氧化锌、氧化锌晶须、氧化锑、铅白、水合氧化锡、氯化银、硫酸钙、硫酸钡、硫酸镁、碳酸钙、碳酸镁、氢氧化锌、氢氧化镁、氢氧化钙、氢氧化铝、硬脂酸钙、硬脂酸锌、硬脂酸镁、棕榈酸钾、山嵛酸镁、滑石粉、石棉、碳纳米管、碳化硅、水滑石、金属微球、绢云母、云母、蛭石、伊利石、蒙皂石、蒙脱石、锂蒙脱石、双氢氧化物、沸石、叶腊石、硅灰石、纳米层状硅酸盐、纳米级氧化铝、勃姆石、蛇纹石、水铝钙石、海泡石、白云石、硬硅钙石、硅石-矾土、矾土、膨润土、蒙脱土、锂蒙脱土、合成云母及相关改性处理产品。
本发明中,为了使聚酰胺组合物具有更为优良的机械性能,可采用偶联剂对无机填料进行功能性处理,其中偶联剂选自异氰酸酯系化合物、有机硅烷系化合物、有机钛酸酯系化合物、有机硼烷系化合物、环氧化合物,优选为有机硅烷系化合物。
其中,所述有机硅烷系化合物选自含有环氧基的烷氧基硅烷化合物、含有巯基的烷氧基硅烷化合物、含有脲基的烷氧基硅烷化合物、含有异氰酸酯基的烷氧基硅烷化合物、含有氨基的烷氧基硅烷化合物、含有羟基的烷氧基硅烷化合物、含有碳-碳不饱和基的烷氧基硅烷化合物、含有酸酐基的烷氧基硅烷化合物的一种或几种;所述含有环氧基的烷氧基硅烷化合物选自γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基三乙氧基硅烷、β-(3,4-环氧环己基) 乙基三甲氧基硅烷的一种或几种;所述含有巯基的烷氧基硅烷化合物选自γ-巯基丙基三甲氧基硅烷和/或γ-巯基丙基三乙氧基硅烷;所述含有脲基的烷氧基硅烷化合物选自γ-脲基丙基三乙氧基硅烷、γ-脲基丙基三甲氧基硅烷、γ-(2-脲基乙基)氨基丙基三甲氧基硅烷的一种或几种;所述含有异氰酸酯基的烷氧基硅烷化合物选自γ-异氰酸酯基丙基三乙氧基硅烷、γ-异氰酸酯基丙基三甲氧基硅烷、γ-异氰酸酯基丙基甲基二甲氧基硅烷、γ-异氰酸酯基丙基甲基二乙氧基硅烷、γ-异氰酸酯基丙基乙基二甲氧基硅烷、γ-异氰酸酯基丙基乙基二乙氧基硅烷、γ-异氰酸酯基丙基三氯硅烷的一种或几种;所述含有氨基的烷氧基硅烷化合物选自γ-(2-氨基乙基)氨基丙基甲基二甲氧基硅烷、γ-(2-氨基乙基)氨基丙基三甲氧基硅烷、γ-氨基丙基三甲氧基硅烷的一种或几种;所述含有羟基的烷氧基硅烷化合物选自γ-羟基丙基三甲氧基硅烷和/或γ-羟基丙基三乙氧基硅烷;所述含有碳-碳不饱和基的烷氧基硅烷化合物选自γ-甲基丙烯酰氧基丙基三甲氧基硅烷、乙烯基三甲氧基硅烷、N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷盐酸盐的一种或几种;所述含有酸酐基的烷氧基硅烷化合物选自3-三甲氧基甲硅烷基丙基琥珀酸酐;所述有机硅烷系化合物优选为γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-(2-氨基乙基) 氨基丙基甲基二甲氧基硅烷、γ-(2-氨基乙基)氨基丙基三甲氧基硅烷、γ-氨基丙基三甲氧基硅烷或3-三甲氧基甲硅烷基丙基琥珀酸酐。
所述偶联剂的用量为无机填料重量的0.05~10wt%,优选为0.15wt%;当偶联剂的用量小于0.05wt%时,无机填料容易发生凝聚,并且在聚酰胺树脂中分散不良的风险,最终导致机械性能发生下降。
本发明中,所述添加剂包括抗氧剂、阻燃剂、润滑剂、脱模剂、成核剂、着色剂、增塑剂、增韧剂、抗静电剂、增溶剂、分散剂、稳定剂、流动改性剂或其他聚合物树脂中的一种或多种。上述添加剂均为本领域常用的助剂,根据组合物性能要求进行添加。
本发明中,所述抗氧剂包括胺类抗氧剂、酚类抗氧剂、酯类抗氧剂。
胺类抗氧剂包括但不仅限于对异丙氧基二苯胺;4,4-(双α,α-二甲基苄基)二苯胺、N,N- 双(1,4-二甲基戊基)对苯二胺、N,N-二-β-萘基对苯二胺、N-(1,3-二甲基丁基)-N-苯基对苯二胺、2,2,4-三甲基-1,2二氢化喹啉聚合体等。
酚类抗氧剂包括但不仅限于1-羟基-3-甲基-4-异丙基苯、2,4,6-三叔丁基苯酚、β-(4-羟基 -3,5-二叔丁基苯基)丙酸正十八碳醇酯、四[3-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯等。
酯类抗氧剂包括但不仅限于β-(4-羟基-3,5-二叔丁基苯基)丙酸正十八碳醇酯、硫代二丙酸二月桂酯、β,β-硫代二丁酸十八酯、亚磷酸三苯酯、三(2,4-二叔丁基苯基)亚磷酸酯等。
本发明中,所述阻燃剂包括卤系阻燃剂和无卤阻燃剂,所述卤系阻燃剂包括但不仅限于六溴环十二烷、十溴二苯醚、八溴二苯醚、四溴双酚A、双(三溴苯氧基)乙烷、双(五溴苯氧基)乙烷、四溴双酚A环氧树脂、四溴双酚A碳酸酯、亚乙基双(四溴邻苯二甲酰)亚胺、亚乙基双五溴联苯、三(三溴苯氧基)三嗪、双(二溴丙基)四溴双酚A、双(二溴丙基)四溴双酚S、溴化聚苯醚(包括聚(二)溴苯醚等)、溴化聚苯乙烯(包括聚二溴苯乙烯、聚三溴苯乙烯、交联溴化聚苯乙烯等)、溴化交联芳香族聚合物溴化环氧树脂、溴化苯氧基树脂、溴化苯乙烯-马来酸酐共聚物、四溴双酚S、三(三溴新戊基)磷酸酯、聚溴三甲基苯基茚满及三(二溴丙基)异氰脲酸酯等。作为卤系阻燃剂,从挤出或成型等熔融加工时的腐蚀性气体的产生量低、以及表现阻燃性、韧性及刚性等机械物性的观点考虑,优选溴化聚苯醚(包括聚(二)溴苯醚等)、溴化聚苯乙烯(包括聚二溴苯乙烯、聚三溴苯乙烯、交联溴化聚苯乙烯等),更优选溴化聚苯乙烯。其中,溴化聚苯乙烯中的溴含量优选为55wt%~75wt%。
所述无卤阻燃剂选自含氮阻燃剂、含膦阻燃剂或含氮和膦的阻燃剂的一种或几种;优选为含膦阻燃剂。所述含磷阻燃剂包括但不仅限于红磷、单磷酸芳基磷酸酯、双膦酸芳基磷酸酯、烷基膦酸二甲酯、膦酸三苯酯、膦酸三甲苯酯、膦酸三(二甲苯)酯、丙苯系膦酸酯、丁苯系膦酸酯或次膦酸盐的一种或几种;优选为次膦酸盐;次膦酸盐以如下式(I)和/或(II)表示的化合物为代表。
在式(I)及式(II)中,R及R可以相同,也可以不同,分别表示直链状或分支状的C1~C6- 烷基、芳基或苯基。R3表示直链状或分支状的C1~C10-亚烷基、C6~C10-亚芳基、C6~C10-烷基亚芳基、或C6~C10芳基亚烷基。M表示钙原子、镁原子、铝原子和/或锌原子。m是2或3, n是1或3,x是1或2。
次膦酸盐化合物的更具体例子包括但不仅限于二甲基次膦酸钙、二甲基次膦酸镁、二甲基次膦酸铝、二甲基次膦酸锌、乙基甲基次膦酸钙、乙基甲基次膦酸镁、乙基甲基次膦酸铝、乙基甲基次膦酸锌、二乙基次膦酸钙、二乙基次膦酸镁、二乙基次膦酸铝、二乙基次膦酸锌、甲基正丙基次膦酸钙、甲基正丙基次膦酸镁、甲基正丙基次膦酸铝、甲基正丙基次膦酸锌、甲烧二(甲基次膦酸)钙、甲烷二(甲基次膦酸)镁、甲烷二(甲基次膦酸)铝、甲烷二(甲基次膦酸) 锌、苯-1,4-(二甲基次膦酸)钙苯-1,4-(二甲基次膦酸)镁、苯-1,4-(二甲基次膦酸)铝、苯-1,4-(二甲基次膦酸)锌、基苯基次膦酸钙、甲基苯基次膦酸镁、甲基苯基次膦酸铝、甲基苯基次膦酸锌、二苯基次膦酸钙、二苯基次膦酸镁、二苯基次膦酸铝、二苯基次膦酸锌等,优选二甲基次膦酸钙、二甲基次膦酸铝、二甲基次膦酸锌、乙基甲基次膦酸丐、乙基甲基次膦酸铝、乙基甲基次膦酸锌、二乙基次膦酸钙、二乙基次膦酸铝、二乙基次膦酸锌,更优选二乙基次膦酸铝。
作为阻燃剂的次膦酸盐化合物可容易地从市场获得。可从市场获得的次膦酸盐化合物的例子包括科莱恩公司(Clariant)制造的EXOLIT OP11230、0P1311、0P1312、0P930、P935等。
其中,在使用次膦酸盐或二膦氧化物时,优选并用聚磷酸三聚氰胺类作为磷类阻燃剂。通过并用聚磷酸三聚氰胺类,在阻燃性试验时可以促进聚酰胺的碳化、缩短燃烧时间。若使用过量的聚磷酸三聚氰胺类,将聚酰胺组合物注射成型时,有产生模具污染等不良问题的趋势,因此优选聚磷酸三聚氰胺类的量相对于聚酰胺100质量份小于1质量份。
所述含氮阻燃剂包括但不仅限于三聚氰胺、三聚氰胺氰脲酸盐、三聚氰胺硫酸盐、三聚氰胺硼酸盐、三聚氰胺草酸盐、三聚氰胺磷酸盐(三聚氰胺磷酸二氢盐、三聚氰胺磷酸氢盐) 或三聚氰胺焦磷酸二氢盐、新戊二醇硼酸三聚氰胺、胍及其本领域技术人员已知的衍生物,以及聚合的三聚氰胺磷酸盐、多磷酸铵、三羟基乙基异氰脲酸酯(任选地还为以与三羟基乙基异氰脲酸酯的混合物的形式的多磷酸铵)。
为进一步提高阻燃剂的阻燃效果,本发明中可选择阻燃剂与阻燃助剂的组合物,作为阻燃助剂包括但不仅限于三氧化锑、四氧化二锑、五氧化二锑、等氧化锑类;氧化铁、γ-氧化铁等氧化铁类;氧化钠、一氧化锡、二氧化锡、氧化锌、氧化铝(矾土)、氧化铝(勃姆石)、二氧化钛、氧化钙、氧化锆、氧化锰、氧化钼、氧化钴、氧化铋、氧化铬、氧化锡、氧化镍、氧化铜及氧化钨等金属氧化物类;铝、铁、钛、锰、锌、钼、钴、铋、铬、锡、锑、镍、铜及钨等金属粉末;碳酸锌、碳酸钙、碳酸镁及碳酸钡等金属碳酸盐;硼酸锌、硼酸镁、硼酸钙及硼酸铝等金属硼酸盐;氢氧化镁、氢氧化钙、氢氧化铝、高岭土、粘土、锡酸锌、锑酸钠、二氧化硅(硅石)等。它们可以单独使用或将2种以上组合来使用。这些阻燃助剂可以用偶联剂处理,诸如硅烷偶联剂、钛偶联剂等。其中,优选锡酸锌、锑酸钠和/或硼酸锌。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包含至多50wt%的一种或多种抗冲击改性剂。所述冲击改性剂包括但不局限于结晶性烯烃聚合物、天然橡胶、乙烯- α-烯烃共聚物、乙烯-丙烯酸酯共聚物、聚丁二烯、聚异戊二烯、聚异丁烯、丁二烯和/或异戊二烯与苯乙烯或与苯乙烯衍生物和/或与其它共聚单体的共聚物、氢化共聚物、和/或通过接枝或与酐、(甲基)丙烯酸或其酯共聚而制得的共聚物。所述冲击改性剂可以是具有交联弹性体芯的接枝橡胶,所述交联弹性体芯由丁二烯、异戊二烯或烷基丙烯酸酯构成,并且具有由聚苯乙烯构成的接枝壳,或者可以是非极性或极性烯烃均聚物或共聚物,例如乙丙橡胶,乙烯-丙烯二烯烃橡胶,或乙烯-辛烯橡胶,或乙烯-乙酸乙烯酯橡胶,或通过接枝或与酐、(甲基) 丙烯酸或其酯共聚而得到的非极性或极性烯烃均聚物或共聚物;所述冲击改性剂还可以是羧酸官能化的共聚物,例如聚(乙烯-共-(甲基丙烯酸)或聚(乙烯-1-烯烃-共(甲基)丙烯酸),其中 1-烯烃是链烯烃或者具有多于4个原子的不饱和(甲基)丙烯酸酯,包括酸基团被金属离子中和到一定程度的那些共聚物。其中,所述抗冲击改性剂还优选为离子聚合物,其中聚合物键合的羧基通过金属离子全部相互键合或键合到一定程度。
基于苯乙烯单体(苯乙烯和苯乙烯衍生物)和其它乙烯基芳族单体的冲击改性剂,是由链烯基芳族化合物和共轭二烯烃构成的嵌段共聚物,和由链烯基芳族化合物和共轭二烯烃构成的氢化嵌段共聚物,以及这些类型冲击改性剂的组合。可以与苯乙烯一起使用或以与苯乙烯的混合物形式使用的其它链烯基芳族化合物是在芳环和/或在C=C双键上被C1~C20烃基或被卤原子取代的乙烯基芳族单体。链烯基芳族单体的实例是苯乙烯、对甲基苯乙烯、α-甲基苯乙烯、乙基苯乙烯、叔丁基苯乙烯、乙烯基甲苯、1,2-二苯基乙烯、1,1-二苯基乙烯、乙烯基二甲苯、乙烯基甲苯、乙烯基萘、二乙烯基苯、溴代苯乙烯、和氯代苯乙烯及其组合。优选苯乙烯、对甲基苯乙烯、α-甲基苯乙烯、乙烯基萘叔丁基苯乙烯、乙烯基甲苯、1,2-二苯基乙烯、1,1-二苯基乙烯或这些物质的混合物。
可以使用的二烯烃单体的实例是1,3-丁二烯、2-甲基-1,3-丁二烯、2,3-二甲基-1,3-丁二烯、 1,3-戊二烯、1,3-己二烯、异戊二烯、氯丁二烯和间戊二烯。优选1,3-丁二烯和异戊二烯,尤其是1,3-丁二烯(下文中以缩写形式丁二烯表示)。所使用的链烯基芳族单体优选包括苯乙烯,所使用的二烯烃单体优选包括丁二烯,这意味着优选苯乙烯-丁二烯嵌段共聚物。
除了苯乙烯单体和二烯烃单体以外,还可以同时使用其它另外的单体。合适的共聚单体的实例分别是丙烯酸酯,尤其是丙烯酸C1~C12烷基酯,例如丙烯酸正丁酯或丙烯酸2-乙基己酯,和甲基丙烯酸酯,尤其是甲基丙烯酸C1~C12烷基酯,例如甲基丙烯酸甲酯(MMA)。其它可能的共聚单体是(甲基)丙烯腈、(甲基)丙烯酸缩水甘油酯、乙烯基甲基醚、二元醇的二烯丙基和二乙烯基醚、二乙烯基苯和乙酸乙烯酯。
特别优选马来酸酐接枝官能化的丁二烯与苯乙烯的共聚物,通过与马来酸酐接枝制得的非极性或极性烯烃均聚物和共聚物、以及羧酸官能化的共聚物,例如聚(乙烯-共(甲基)丙烯酸) 或聚(乙烯-共-1-烯烃-共(甲基)丙烯酸),其中所述酸基团已在一定程度上被金属离子中和。可以用于所述添加剂组分的可市购的冲击改性剂实例有:
TAFMER MC201:g-MA(0.6%)67%EP共聚物(20mo1%丙烯)+33%EB共聚物(15mo1%1- 丁烯)的共混物:Mitsui Chemicals,日本。
TAFMER MH5010:g-MA(0.6%)乙烯-丁烯共聚物:Mitsui。
TAFMER MH7010:g-MA(0.6%)乙烯-丁烯共聚物:Mitsui。
TAFMER MH7020:g-MA(0.7%)EP共聚物:Mitsui。
EXXELOR VA1801:g-MA(0.7%)EP共聚物:Exxon Mobile Chemicals,US。
EXXELOR VA1803:g-MA(0.5-0.9%)EP共聚物,无定形,Exxon。
EXXELOR VA1810:g-MA(0.5%)EP共聚物,Exxon。
EXXELOR MDEX 9411:g-MA(0.7%)EPDM,Exxon。
FUSABOND MN4930:g-MA(0.5%)乙烯-辛烯共聚物,DuPont,US。
FUSABOND EB560D:g-MA乙烯-丙烯酸正丁酯共聚物,DuPont ELVALOY,DuPont。
除了共轭二烯烃之外,如果合适的话,氢化嵌段共聚物还包含低级烃部分,例如乙烯、丙烯、1-丁烯、二环戊二烯或非共轭二烯烃。氢化嵌段共聚物包括但不仅限于通过苯乙烯-丁二烯共聚物的氢化和苯乙烯-丁二烯-苯乙烯共聚物的氢化,得到氢化嵌段共聚,即苯乙烯-(乙烯-丁烯)双嵌段共聚物和苯乙烯-(乙烯-丁烯)-苯乙烯三嵌段共聚物。合适的氢化嵌段共聚物是可以从市场上购得的产品,例如(Kraton聚合物)G1650、G1651和G1652,以及(Asahi Chemicals)H1041、H1043、H1052、H1062、H1141和H1272。
非氢化嵌段共聚物的实例是聚苯乙烯-聚丁二烯、聚苯乙烯-聚(乙烯-丙烯)聚苯乙烯-聚异戊二烯、聚(α-甲基苯乙烯)-聚丁二烯、聚苯乙烯-聚丁二烯-聚苯乙烯(SBS)、聚苯乙烯-聚(乙烯-丙烯)-聚苯乙烯、聚苯乙烯-聚异戊二烯-聚苯乙烯、和聚(α-甲基苯乙烯)聚丁二烯-聚(α- 甲基苯乙烯)及其组合。可以从市场上购得的合适的非氢化嵌段共聚物有商标为(Phillips)、 (Shell)、(Dexco)和(Kuraray)的多种产品。
结晶性烯烃聚合物的实例是低密度、中密度和高密度聚乙烯、聚丙烯、聚丁二烯、聚-4- 甲基戊烯、乙烯-丙烯嵌段共聚物、或乙烯-丙烯无规共聚物、乙烯-甲基己二烯共聚物、丙烯- 甲基己二烯共聚物、乙烯-丙烯丁烯共聚物乙烯丙烯己烯共聚物、乙烯-丙烯-甲基己二烯共聚物、聚(乙烯-乙酸乙烯酯)(EVA)、聚(乙烯-丙烯酸乙酯)(EEA)、乙烯辛烯共聚物、乙烯-丁烯共聚物、乙烯己烯共聚物乙烯丙烯二烯烃三元共聚物,以及上述聚合物的组合。
优选地,上述抗冲击改性剂包含具有基团的成分,这些通过主链聚合物与不饱和二酸酐、与不饱和二羧酸、或与不饱和二羧酸的单烷基酯的热反应或自由基反应,以足以与聚酰胺良好结合的浓度引入,并且此处优选的是使用选自以下的试剂:
马来酸、马来酸酐、马来酸单丁酯、富马酸、乌头酸和/或衣康酸酐。优选0.1~4.0wt%的不饱和酸酐接枝到作为C的成分的抗冲击组分上,或者不饱和二酸酐或其前体通过与其它不饱和单体一起接枝来施加。通常优选接枝度为0.1~1.0%,特别优选为0.3~0.7%。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包含在多色成型或聚合物合金中使用的其它材料,使用的其它树脂诸如低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、聚丙烯、乙烯/丙烯共聚物、乙烯/丁烯共聚物、乙烯/乙酸乙烯酯共聚物、乙烯/乙酸乙烯酯共聚物的皂化物、乙烯/丙烯酸共聚物、乙烯/甲基丙烯酸共聚物、乙烯/丙烯酸甲酯共聚物、乙烯/甲基丙烯酸甲酯共聚物、乙烯/丙烯酸乙酯共聚物、聚丁二烯、乙烯/丙烯/二烯共聚物、聚苯乙烯等聚烯烃系树脂;聚对苯二甲酸丁二醇酯、聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯、聚萘二甲酸丁二醇酯、聚间苯二甲酸乙二醇酯、多芳基化合物、液晶聚酯等聚酯系树脂;聚缩醛、聚苯醚等聚醚树脂;聚砜、聚醚砜等聚砜树脂;聚苯硫醚、聚硫醚砜等聚硫醚系树脂;聚醚醚酮、聚烯丙基醚酮等聚酮系树脂;聚丙烯腈、聚甲基丙烯腈、丙烯腈/苯乙烯共聚物、丙烯腈/丁二烯/苯乙烯共聚物、甲基丙烯腈/丁二烯/苯乙烯共聚物等的聚腈系树脂;聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯等聚甲基丙烯酸酯系树脂;聚乙酸乙烯酯等聚乙烯酯系树脂;聚偏氯乙烯、聚氯烯氯乙烯/偏氯乙烯共聚物、偏氯乙烯/丙烯酸甲酯共聚物等的聚氯乙烯系树脂;乙酸纤维素、丁酸纤维素等纤维素系树脂;聚偏氟乙烯、聚氟乙烯、乙烯/四氟乙烯共聚物、聚氯三氟乙烯、乙烯/氯三氟乙烯共聚物、四氟乙烯/六氟丙烯共聚物、四氟乙烯 /六氟丙烯/偏氟乙烯共聚物等氟系树脂;聚碳酸酯等聚碳酸酯系树脂;热塑性聚酰亚胺、聚酰胺酰亚胺、聚醚酰亚胺等聚酰亚胺系树脂;热塑性聚氨酯树脂。
本发明所述聚酰胺树脂的聚酰胺组合物中,应用于多色成型或聚合物合金中聚合物材料还包括脂肪族聚酰胺和/或半芳香族聚酰胺,诸如源自4-20个碳原子的脂肪族二酸和脂肪族二胺,或者4-20个碳原子的内酰胺,或者4-20个碳原子的脂肪族二酸、脂肪族二胺和内酰胺的聚合物中的一种或多种。包括但不仅限于,聚己二酰己二胺(PA66)、聚内酰胺(PA6)、聚癸二酰己二胺(PA610)、聚酰胺612、聚癸二酰癸二胺(PA1010)、己二酸一己二胺一己内酰胺共聚物(PA66/6)、聚十一内酰胺(PA11)、聚十二内酰胺(PA12),及其两种或多种的混合物。半芳香族聚酰胺诸如聚己二酰间亚苯基二甲胺(MXD6)、聚亚己基对苯二甲酰胺(PA6T)、聚亚壬基对苯二甲酰胺(PA9T)、聚亚癸基对苯二甲酰胺(PA10T)、聚十二甲撑对苯二甲酰胺(PA12T)、聚双(4-氨基环基)甲烷十二酰胺(PACM12)或形成它们的聚酰胺原料单体和/或使用多种上述聚酰胺原料单体得到的共聚物等聚酰胺系树脂等。除上述聚酰胺外,还包括非晶聚酰胺,所述非晶聚酰胺包括但不仅限于间苯二甲酸/对苯二甲酸/1,6-己二胺/双(3-甲基-4-氨基环己基)甲烷的缩聚物、对苯二甲酸/2,2,4-三甲基-1,6-己二胺/2,4,4-三甲基-1,6-己二胺的缩聚物、间苯二甲酸/双(-甲基-4-氨基环己基)甲烷/-十二内酰胺的缩聚物、间苯二甲酸/对苯二甲酸/1,6己二胺的缩聚物、间苯二甲酸/2,2,4-三甲基-1,6-己二胺/2,4,4-三甲基-1,6-己二胺的缩聚物、间苯二甲酸/对苯二甲酸/2,2,4-三甲基-1,6-己二胺/2,4,4-三甲基-1,6己二胺的缩聚物、间苯二甲酸/对苯二甲酸/其它二胺成分的缩聚物,或形成它们的聚酰胺原料单体和/或使用多种上述聚酰胺原料单体得到的共聚物等聚酰胺系树脂等。通过添加非晶性聚酰胺,可以是表面光泽性等提高。
本发明所述聚酰胺树脂的聚酰胺组合物中,应用于多色成型或聚合物合金中聚合物材料还包括聚苯醚(PPE)。合适的聚苯醚包括但不仅限于聚(2,6-二乙基-1,4-亚苯基)醚、聚(2-甲基 -6-乙基-1,4-亚苯基)醚、聚(2-甲基-6-丙基-1,4-亚苯基)醚、聚(2,6-二丙基-1,4-亚苯基)醚、聚(2- 乙基-6-丙基-1,4-亚苯基)醚或诸如包含2,3,6-三甲基酚的共聚物、以及聚合物的混合物。优选任选地与2,3,6-三甲基酚单元组合的聚(2,6-二甲基-1,4-亚苯基)醚。可以以均聚物、共聚物、接枝共聚物、嵌段共聚物或离聚物的形式使用聚苯醚。为了更好的可相容性,使用处于多官能化合物形式的、与聚苯醚、聚酰胺或二者相互作用的增容剂。所述相互作用可以是化学作用(例如通过接枝)和/或物理作用(例如通过对分散相的表面性能的影响)。
为改善树脂和/或抗冲改性剂与聚酰胺树脂的相容性,本发明中可添加不超过15%质量分数的增溶剂,所述增溶剂可以是含有至少一个羧酸基团、羧酸酐基团、酯基团、酰胺基团或酰亚胺基团的多官能化合物。诸如马来酸、马来酸酐、2-甲基马酸酐、2-氯马来酸酐、2,3-二基马来酸酐、二环[2,2,1]-5-庚烯-2,3-二羧酸酐、4-甲基-4-环已烯-1,2-二羧酸酐、二环(2.2.2) 辛-5-烯-2,3-二羧酸酐、1,2,3,4,5,8,9,10-八氢萘-2,3-二羧酸酐、2-氧-1,3-二酮螺(4.4)壬-7-烯、二环(2.2.1)庚-5-烯-2,3-二羧酸酐、马来海松酸酐、邻苯二甲酸酐、柠康酸酐、富马酸、巴豆酸、中康酸、丙烯酸、甲基丙烯酸、乙基丙烯酸、甲基马来酸、甲基马来酸酐、衣康酸、衣康酸酐、丁烯基琥珀酸、丁烯基琥珀酸酐、四氢邻苯二甲酸、四氢邻苯二甲酸酐、N-苯基马来酰亚胺、柠檬酸、苹果酸、降冰片-5-烯-2,3-二羧酸酐、纳迪克酸酐(nadic anhydride)、甲基纳迪克酸酐、纳迪克酸酐(himic anhydride)、甲基纳迪克酸酐、以及x-甲基-二环(2.2.1)庚-5-烯2,3- 二羧酸酐(XMNA)、2-羟基十九烷-1,2,3-三羧酸和上述酸与C1~C12醇(例如甲醇或乙醇)的单酯或二酯、上述酸的单酰胺或二酰胺(如果合适,可以在N上取代具有至多12个碳原子的烷基或芳基)以及与碱金属或碱土金属(例如钙和钾)的盐。其中,优选马来酸、富马酸、马来酸酐和柠檬酸。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包含按重量份计,0-20 份的多元醇。所述的多元醇包括二元醇、三元醇、羟基数量大于等于四的多元醇、聚多元醇中的至少一种。所述的二元醇包括但不仅限于1,2-乙二醇、1,3-丙二醇、2,3-丁二醇、1,5-戊二醇、2,2-二甲基-1,3-丙二醇、聚醚二醇类中的至少一种;所述的三元醇包括但不仅限于甘油、三羟甲基丙烷、2,3-二(2′-羟乙基)环己烷-1-醇、1,2,6-己三醇、1,1,1三-(羟甲基)乙烷、3-(2′ -羟乙氧基)丙烷-1,2-二醇、3-(2′-羟丙氧基)丙烷-1,2-二醇、2-(2'-羟乙氧基)烷-1,2-二醇、6-(2′ -丙氧基)已烷-1,2-二醇、1,1,1-三[(2′-羟乙氧基)甲基]乙烷、1,1,1-三[(2′-羟丙氧基)甲基]丙烷、 1,1,1-三(4′-羟苯基)乙烷、1,1,1-三(羟苯基)丙烷、1,1,5-三(羟苯基)-3-甲基戊烷、三羟甲基丙烷乙氧基化物、三羟甲基丙烷丙氧基化物和三羟基聚醚类化合物(如二甘醇、三甘醇)中的至少一种;所述的羟基数量大于等于四的多元醇和/或聚合物包括但不限于1,1,3-三(二羟基-3- 甲基苯基)丙烷、1,1,4-三(二羟基苯基)丁烷、二(三羟甲基丙烷)、1,1,3,3-四(甲氧基)丙烷、季戊四醇、双季戊四醇、三季戊四醇和具有一定聚合度的聚乙烯醇、乙烯乙烯醇共聚物、树枝状超支化聚酯,以及上述多元醇的组合。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包含润滑剂,润滑剂包括但不仅限于硬脂酸钙、硬脂酸钠、硬脂酸锌、硬脂酸锂、褐煤酸钙、单硬脂酸甘油酯、三硬脂酸甘油酯、乙撑双硬脂酰胺、乙撑双月桂酰胺、乙撑双油酸酰胺、低分子量离聚物、乙烯- 丙烯酸共聚物、乙烯-醋酸乙烯共聚物、聚乙烯蜡、氧化聚乙烯、脂肪酸酰胺、季戊四醇四硬脂酸酯及其组合。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包含热稳定剂,其包含铜类稳定剂、酚类稳定剂、亚磷酸酯类稳定剂、受阻胺类稳定剂、含硫稳定剂、无机含磷稳定剂、草酸苯胺系稳定剂、芳香族仲胺系稳定剂、炭黑、金属粉末及其组合。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包含铜化合物,铜化合物包括但不仅限于有机或无机酸、一元或二元酚的一价或二价铜盐,磷酸铜、焦磷酸铜、硫酸铜和硝酸铜,氧化铜或氧化亚铜,铜盐与胺、酰胺、内酰胺、氰化物或膦的络合物,一价或二价铜的卤化物,一价或二价铜的脂肪酸铜盐。特别优选一价铜化合物,碘化亚铜、氯化亚铜、溴化亚铜、乙酸铜、脂肪酸铜、氧化亚铜,二价铜化合物氯化铜、溴化铜、碘化铜、硫酸铜、氧化铜。
本发明聚酰胺组合物可优选包含一种用量为铜化合物的重量的1至20倍的碱金属卤化物。碱金属卤化物包括但不仅限于氯化锂、溴化锂、碘化锂、氟化钠、氯化纳、溴化钠、碘化钠、氟化钾、氯化钾、溴化钾和碘化钾。它们当中,优选碘化钾。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括酚类稳定剂,作为酚类稳定剂,没有特别限制,可以举例:受阻酚类化合物。受阻酚类化合物包括但不仅限于N,N’ -己烷-1,6-二基双[3-(3,5-二叔丁基-4-羟基苯基丙酰胺)]、季戊四醇四[3-(3,5-二叔丁基-4-羟基苯基)丙酸酯]、N,N’-六亚甲基双(3,5-二叔丁基-4-羟基氢化肉桂酰胺)、三乙二醇双[3-(3-叔丁基 -5-甲基-4-羟基苯基)丙酸酯]、3,9-双{2-[3-(3-叔丁基-4羟基-5-甲基苯基)丙炔氧基]-1,1-二甲基乙基}-2,4,8,10-四氧杂螺[5.5]十一烷、3,5-二叔丁基-4-羟基苄基膦酸二乙酯、1,3,5-三甲基-2,4,6- 三(3,5-二叔丁基-4-羟基苄基)苯、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)异氰脲酸等。
这些酚类稳定剂可以使用一种也可以两种以上组合使用。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括亚磷酸酯类稳定剂,没有特别限制,可以列举例如:亚磷酸三辛酯、亚磷酸三月桂酯、亚磷酸三癸酯、亚磷酸二苯辛酯、亚磷酸三异癸酯、亚磷酸一苯二异癸酯、亚磷酸一苯二(十三烷基)酯、亚磷酸二苯异辛酯、亚磷酸二苯异癸酯、亚磷酸二苯(十三烷基)酯、亚磷酸三苯酯、亚磷酸三(壬基苯基) 酯、亚磷酸三(2,4-二叔丁基苯基)酯、亚磷酸三(2,4-二叔丁基-5-甲基苯基)酯、亚磷酸三(氧基乙基)酯、4,4’-丁叉-双(3-甲基-6-叔丁基苯基四(十三烷基))二亚磷酸酯、四(C12~C15混合烷基)-4,4’-异丙叉二苯基二亚磷酸酯、4,4’-异丙叉双(2-叔丁基苯基)·二(壬基苯基)亚磷酸酯、亚磷酸三(联苯基)酯、四(十三烷基)-1,1,3-三(2-甲基-5-叔丁基-4-羟基苯基)丁烷二亚磷酸酯、四(十三烷基)-4,4’-丁叉双(3-甲基-6-叔丁基苯基)二亚磷酸酯、(C1~C15混合烷基)-4,4’-异丙叉二苯基二亚磷酸酯、三(单-、二-混合壬基苯基)亚磷酸酯、4,4’-异丙叉双(2-叔丁基苯基)·二 (壬基苯基)亚磷酸酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、三(3,5-二叔丁基-4-羟基苯基) 亚磷酸酯、氢化4,4’-异丙叉二苯基聚亚磷酸酯、双(辛基苯基)·双(4,4’-丁叉基双(3-甲基-6- 叔丁基苯基))·1,6-己醇二亚磷酸酯、六(十三烷基)-1,1,3-三(2-甲基-4-羟基-5-叔丁基苯基)丁烷三亚磷酸酯、三(4,4’异丙叉双(2-叔丁基苯基)亚磷酸酯、三(1,3-硬脂酰氧异丙基)亚磷酸酯、 2,2-亚甲基双(4,6-二叔丁基苯基)辛基亚磷酸酯、2,2-亚甲基双(3-甲基-4,6-二叔丁基苯基)-2-乙基基亚磷酸酯、四(2,4-二叔丁基-5-甲基苯基)-4,4’-联苯撑二亚磷酸酯以及四(2,4-二叔丁基苯基)-4,4’-联苯撑二亚磷酸酯等。这些亚磷酸酯类稳定剂可以使用一种,也可以两种以上组合使用。
作为亚磷酸酯类稳定剂,也可以列举季戊四醇型亚磷酸酯化合物。作为季戊四醇型亚磷酸酯化合物,可以列举例如:2,6-二叔丁基-4-甲基苯基·苯基·季戊四醇二亚磷酸酯、2,6- 二叔丁基-4-甲基苯基·甲基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基-2-乙基己基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基异癸基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4- 甲基苯基·月桂基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·异十三烷基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·硬脂基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4- 甲基苯基·环己基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基苄基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·乙基溶纤剂·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·丁基卡必醇·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·辛基苯基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·壬基苯基·季戊四醇二亚磷酸酯、双(2,6-二叔丁基-4- 甲基苯基)季戊四醇二亚磷酸酯、双(2,6-二叔丁基-4-乙基苯基)季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·2,6-二叔丁基苯基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·2,4- 二叔丁基苯基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·2,4-二叔辛基苯基·季戊四醇二亚磷酸酯、2,6-二叔丁基-4-甲基苯基·2-环己基苯基·季戊四醇二亚磷酸酯、2,6-二叔戊基-4-甲基苯基苯基·季戊四醇二亚磷酸酯、双(2,6-二叔戊基-4-甲基苯基)季戊四醇二亚磷酸酯以及双2,6-二叔辛基-4-甲基苯基)季戊四醇二亚磷酸酯等。
这些季戊四醇型亚磷酸酯类稳定剂可以使用一种,也可以两种以上组合使用。作为季戊四醇型亚磷酸酯化合物,优选双(2,6-二叔丁基-4-甲基苯基)季戊四醇二亚磷酸酯、双(2,6-二叔丁基-4-乙基苯基)季戊四醇二亚磷酸酯、双(2,6-二叔戊基-4-甲基苯基)季戊四醇二亚磷酸酯以及双(2,6-二叔辛基-4-甲基苯基)季戊四醇二亚磷酸酯等,更优选双(2,6-二叔丁基-4-甲基苯基) 戊四醇二亚磷酸酯。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括合适的位阻胺类稳定剂例如选自癸二酸二(2,2,6,6-四甲基-4-哌啶基)酯,琥珀酸二(2,2,6,6-四甲基-4-哌啶基)酯,癸二酸二(1,2,2,6,6-五甲基-4-哌啶基)酯,癸二酸二(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)酯,正丁基-3,5-二叔丁基-4-羟基基丙二酸二(1,2,2,6,6-五甲基-4-哌啶基)酯,1-(2-羟基乙基)-2,2,6,6-四甲基-4-羟基哌啶和琥珀酸的缩合产物,N,N’-二(2,2,6,6-四甲基-4-哌啶基六亚甲基二胺和1-叔辛氨基-2,6-二氯-1,3,5三嗪的线性或环状缩合物,次氮基三乙酸三(2,2,6,6-四甲基-4-哌啶基) 酯,1,2,3,4-丁烷四甲酸四(2,2,6,6-四甲基-4-哌啶基)酯,4-(乙基氨基甲酰氧基)-2,2,6,6-四甲基哌啶,4-(环己基氨基甲酰氧基)-2,2,6,6-四甲基哌啶,4-(苯基氨基甲酰氧基)-2,2,6,6-四甲基哌啶,双(2,2,6,6-四甲基-4-哌啶基)碳酸酯,双(2,2,6,6-四甲基-4-哌啶基)草酸酯,双(2,2,6,6-四甲基-4哌啶基)丙二酸酯,双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯,双(2,2,6,6-四甲基-4-哌啶基)己二酸酯,双(2,2,6,6-四甲基-4-哌啶基)对苯二甲酸酯,双(2,2,6,6-四甲基--哌啶基)-甲苯-2,4-二氨基甲酸酯,双(2,2,6,6-四甲基-4-哌啶基)-六亚甲基-1,6-二氨基甲酸酯,三(2,2,6,6-四甲基-4-哌啶基)-苯-1,3,5-三甲酸酯,三(2,2,6,6-四甲基-4-哌啶基)-苯-1,3,4-三甲酸酯,1,2-双(2,2,6,6-四甲基-4-啶氧基)-乙烷,α,α-双(2,2,6,6-四甲基-4-哌啶氧基)对二甲苯,1,1’-(1,2-亚乙基)二(3,3,5,5- 四甲基哌嗪酮),4-苯甲酰基-2,2,6,6-四甲基哌啶,4-(苯基乙酰氧基)-2,2,6,6-四甲基哌啶,4- 硬脂氧基-2,2,6,6-四甲基哌啶,丙二酸二(1,2,2,6,6-五甲基哌啶基)-2-正丁基-2-(2羟基-3,5-二叔丁基苄基)酯,3-正辛基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸烷-2,4-二酮,癸二酸二(1-辛氧基-2,2,6,6-四甲基哌啶基)酯,琥珀酸二(1-辛氧基-2,2,6,6-四甲基哌啶基)酯,N,N’-二(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺和4-吗啉代-2,6-二氯-1,3,5-三嗪的线性或环状缩合物,4-甲氧基 -2,2,6,6-四甲基哌啶、4-乙酰氧基-2,2,6,6-四甲基哌啶,2-氯-4,6-二(4-正丁基氨基-2,2,6,6-四甲基哌啶基-1,3,5-三嗪和1,2-二(3-氨基丙基氨基)乙烷的缩合物,2-氯-4,6-二(4-正于基氨基 -1,2,2,6,6-五甲基哌啶基)-1,3,5-三嗪和1,2-二(3-氨基丙基氨基)乙烷的缩合物,8-乙酰基-3-十二烷基-7,7,9,9-四甲基-1,3,8-三氮杂螺[4.5]癸烷-2,4-二酮,3-十二烷基-1-(2,2,6,6-四甲基-4-哌啶基) 吡咯烷-2,5-二酮,3-十二烷基-1-(1,2,2,6,6-五甲基-4-哌啶基)吡咯烷-2,5-二酮,4-硬脂酰氧基 -2,2,6,6-四甲基哌啶,4-丙烯酰氧基-2,2,6,6-四甲基哌啶,4-十六烷氧基-和4-硬脂氧基-2,2,6,6-四甲基哌啶的混合物,4-环氧基-2,2,6,6-四甲基哌啶,4-苄氧基-2,2,6,6-四甲基哌啶,4-苯氧基 -2,2,6,6-四甲基哌啶,N,N’-二(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺和4-环己基氨基-2,6- 二氯-1,3,5-三嗪的缩合物,1,2-二(3-氨基丙基氨基)乙烷、2,4,6-三氯-1,3,5-三嗪和4-丁基氨基 -2,2,6,6-四甲基哌啶的缩合物(CAS号:136504-96-6),1,6-己二胺、2,4,6-三氯-1,3,5-三嗪、N,N- 二丁基胺和4-丁基氨基-2,2,6,6-四甲基哌啶的缩合物(CAS号:192268-61-7),N-(2,2,6,6-四甲基-4-哌啶基)-正十二烷基琥珀酰亚胺,N-(1,2,2,6,6-五甲基-4-哌啶基)-正十二烷基琥珀酰亚胺, 2-十一烷基-7,7,9,9-四甲基-1-氧杂-3,8-二氮杂-4-氧代螺[4,5]癸烷,7,7,9,9-四甲基-2-环十一烷基-1-氧朵-3,8-二氮-4-氧代螺[4,5]癸烷和表氯醇的反应产物,1,1-二(1,2,2,6,6-五甲基-4-哌啶氧基羰基)-2-(4-甲氧基苯基)烯,N,N’-二甲酰基-N,N’-二(2,2,6,6-四甲基-4-哌啶基)六亚甲基二胺,聚[甲基丙基-3-氧基-(2,2,6,6-四甲基-4-哌啶基)]硅氧烷,2,4-二[-(1-环已氧基-2,2,6,6-四甲基哌啶-4-基)-N-丁基氨基]-6-(2-羟基乙基)氨基-1,3,5-三嗪,1-(2-羟基-2-甲基丙氧基)-4-十八烷酰氧基-2,2,6,6-四甲基哌啶,5-(2-乙基己酰基)氧基甲基-3,3,5-三甲基-2-啉酮,Sanduvor(Clariant CAS号:106917-31-1),5-(2-乙基己酰基)氧基甲基-3,3,5-三甲基-2-吗啉酮,2,4-二[(1-环已氧基-2,2,6,6-哌啶-4-基)丁基氨基]-6-氯-s-三嗪与N,N’-二(3-氨基丙基)乙二胺的反应产物,1,3,5- 三(N-环己基-N-(2,2,6,6-四甲基哌嗪-3-酮-4-基)氨基)-s-三嗪,1,3,5-三(N-环己基-N-(1,2,2,6,6- 五甲基哌嗪-3-酮-4-基)氨基)-s三嗪、2,4,6-三(2’-羟基-4’-辛氧基苯基)-1,3,5-三嗪,2-(2’- 羟基-4’-己氧基苯基)-4,6-二苯基-1,3,5-三嗪,2-(2’-羟基-4’-辛氧基苯基)-4,6-二(2’,4’-二甲基苯基)-1,3,5-三嗪,2-(2’,4’-二羟基苯基)-4,6-二(2’,4’-二甲基苯基)-1,3,5-三嗪,2,4- 二(2’-羟基-4’-丙氧基苯基)-6-(2’,4’-二甲基苯基)-1,3,5-三嗪,2-(2-羟基-4-辛氧基苯基)-4,6- 二(4’-甲基苯基)-1,3,5-三嗪,2-(2’-羟基-4’-十二烷氧基苯基)-4,6-二(2’,4’-二甲基苯基)-1,3,5- 三嗪,2,4,6-三(2’-羟基-4’-异丙氧基苯基)-1,3,5-三嗪,2,4,6-三(2’-羟基-4’-正己氧基苯基)-1,3,5-三嗪,2,4,6-三(2’-羟基-4’-乙氧羰基甲氧基苯基)-1,3,5-三嗪。这些稳定剂可以使用一种,也可以两种以上组合使用。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括含硫稳定剂。作为含硫稳定剂,没有特别限制,可以列举例如:双十二烷基硫代二丙酸酯、双十四烷基硫代二丙酸酯、双十八烷基硫代二丙酸酯、季戊四醇四(3-十二烷基硫代丙酸酯)、硫代双(N-苯基-β- 萘基胺)等有机硫代酸系化合物;2-巯基苯并噻唑、2-巯基苯并咪唑、2-巯基甲基苯并咪唑和 2-巯基苯并咪唑的金属盐等巯基苯并咪唑系化合物;二乙基二硫代氨基甲酸的金属盐和二丁基二硫代氨基甲酸的金属盐等二硫代氨基甲酸系化合物以及1,3-双(二甲氨基丙基)-2-硫代脲和三丁基硫代脲等硫代脲系化合物;四甲基秋兰姆单硫化物、四甲基秋兰姆二硫化物、二丁基二硫代氨基甲酸镍、异丙基黄原酸镍、三月桂基三硫代亚磷酸酯等。在这些之中,优选巯基苯并咪唑系化合物、二硫代氨基甲酸系化合物、硫代脲系化合物和有机硫代酸系化合物,进一步优选巯基苯并咪唑系化合物和有机硫代酸系化合物。尤其是,具有硫醚结构的硫醚系化合物由于从被氧化的物质中获取氧而还原,因此可以适合地使用。具体而言,更优选2-巯基苯并咪唑、2-巯基甲基苯并咪唑、双十四烷基硫代二丙酸酯、双十八烷基硫代二丙酸酯、季戊四醇四(3-十二烷基硫代丙酸酯),进一步优选双十四烷基硫代二丙酸酯、季戊四醇四(3- 十二烷基硫代丙酸酯)、2-巯基甲基苯并咪唑,特别优选季戊四醇四(3-十二烷基硫代丙酸酯)。这些含硫稳定剂可以使用一种也可以两种以上组合使用。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括无机含磷稳定剂。作为无机含磷稳定剂,没有特别限制,可以列举例如磷酸类、亚磷酸类及次磷酸类以及磷酸金属盐类、亚磷酸金属盐类及次磷酸金属盐类等;作为磷酸类,亚磷酸类及次磷酸类可以列举例如磷酸、亚磷酸、次磷酸、焦亚磷酸及二亚磷酸等;作为磷酸金属盐类,亚磷酸金属盐类及次磷酸金属盐类,可以列举例如上述磷酸等化合物与元素周期表第1族金属的盐;作为无机含磷稳定剂,优选可溶性化合物,可以列举例如磷酸钠、亚磷酸钠及次磷酸钠,更优选亚磷酸钠及次磷酸钠,进一步优选次磷酸钠;作为无机含磷稳定剂,例如可以是其水合物(优选次磷酸钠的水合物(NaH2PO2·nH2O))。这些无机含磷稳定剂可以使用一种,可以两种以上组合使用。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括草酸苯胺系稳定剂。作为草酸苯胺系稳定剂,可优选列举出4,4’-二辛氧基草酰替苯胺、2,2’-二乙氧基草酰替苯胺、2,2’-二辛氧基-5,5’-二叔丁氧基草酰替苯胺(butoxanilide)、2,2’-双十二烷氧基-5,5’- 二叔丁氧基草酰替苯胺、2-乙氧基-2’-乙基草酰替苯胺、N,N’-双(3-二甲氨基丙基)草酰替苯胺、2-乙氧基-5-叔丁基-2’-乙氧基草酰替苯胺(ethoxanilide)及其与2-乙氧基-2’-乙基-5,4’- 二叔丁氧基草酰替苯胺的混合物、邻甲氧基二取代草酰替苯胺与对甲氧基二取代草酰替苯胺的混合物、邻乙氧基二取代草酰替苯胺与对乙氧基二取代草酰替苯胺的混合物等。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括芳香族仲胺系稳定剂。作为芳香族仲胺系稳定剂,优选具有二苯基胺骨架的化合物、具有苯基萘基胺骨架的化合物和具有二萘基胺骨架的化合物,进一步优选具有二苯基胺骨架的化合物和具有苯基萘基胺骨架的化合物。具体而言,可列举出p,p’-二烷基二苯基胺(烷基的碳原子数为8~14)、辛基化二苯基胺、4,4’-双(α,α-二甲基基)二苯基胺、p(p-甲苯磺酰胺)二苯基胺、N,N’-二苯基对苯二胺、N-苯基-N’-异丙基对苯二胺、N-苯基-N’-(1,3-二甲基丁基)对苯二胺和N-苯基-N’ -(3-甲基丙烯酰氧基-2-羟基丙基)对苯二胺等具有二苯基胺骨架的化合物;N-苯基-1-萘基胺和 N,N’-二-2-萘基对苯二胺等具有苯基基胺骨架的化合物;以及2,2-二萘基胺、1,2-二蔡基胺和 1,1-二萘基胺等具有二萘基胺骨架的化合物。在这些之中,更优选4,4’-双(α,α-二甲基苄基) 二苯基胺、N,N’-二-2-萘基对苯二胺和N,N’-二苯基对苯二胺,特别优选N,N’-二-2-萘基对苯二胺和4,4’-双(α,α-二甲基苄基)二苯基胺。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括流动改性剂。上述流动改性剂为含氟聚合物、PE蜡、EBS、褐煤酸钠盐或钙盐、超支化聚合物中的一种或几种的混合物。
本发明所述聚酰胺树脂的聚酰胺组合物中,添加剂组分还可以包括光稳定剂。在上述耐热聚酰胺组合物中,所述的光稳定剂优选为二苯甲酮化合物或水杨酸酯化合物或苯丙三唑化合物中的一种或几种的混合物。本发明所述组合物的复合步骤可通过本领域已知的任何方法进行,包括但不限于直接挤出、带式挤出、反应挤出、反应注射成型、垂直混合、水平混合、进料混合及其组合。所述方法还可包括一旦将耐热聚酰胺材料复合就对其进行造粒、切块或粒化的步骤。例如,耐热聚酰胺材料可使用水下造粒机或线型造粒机来造粒。
为了获得本发明的成型品,可以将本发明的聚酰胺树脂或组合物通过注射成型、挤出成型、吹塑成型、真空成型、熔融纺丝、膜成型等任意成型方法来成型。本发明的半芳族聚酰胺树脂组合可应用于电子电器、汽车、航空、航天、船舶、家电制品、建筑材料、清洁用品、运动用品、日用品等领域的各种制品。例如,汽车发动机冷却水系部件,特别是散热器水箱的顶部和底部等散热器水箱部件、冷却液储备箱、水管、水泵壳、水泵叶轮、阀等水泵部件等在汽车发动机房内与冷却水接触下使用的部件;发动机进气管路、进气歧管、增压器部件、齿轮、风扇轮、引擎盖、发动机护板、换热器壳、制冷器壳、紧固件、垫片;在电子电器领域,本发明可应用于有源或无源部件或部分模制品、印刷电路板、外壳部件、膜、电线、开关、插头、套管、继电器、电阻、电容、插口、熔断器支持件、继电器、线卷骨架、LC或 LED的外壳、绕组、晶体管、插接器、调节器、集成电路、处理器、散热器、控制器、存储器、感应器、变压器绝缘、适配器外壳、手机电脑结构件、绝缘件、显示背板、鼠标外壳、马达后盖、电子电器安全元件、隔板、嵌条、固定钉、固定销、滑轨、导件、螺丝、螺母、隔离膜;以及开关类、超小型滑动开关、DIP开关、开关的外壳、灯座、捆扎带、连接器、连接器的外壳、连接器的壳、IC插座类、绕线轴、线轴罩、继电器、继电器箱、电容器壳体、马达的内部部件、小型马达壳体、齿轮凸轮、均衡轮、垫片、绝缘体、紧固件、扣、线夹、自行车车轮、小脚印轮、安全帽、端子台、电动工具的外壳起动器的绝缘部分、阻流板、罐、散热器水箱、腔罐、贮液罐、保险丝盒、空气净化器壳体、空调风扇端子的外壳、轮罩、吸排气管、轴承承托、气缸头盖、水管叶轮、离合器分离杆、扬声器振动板、耐热容器、微波炉部件、电饭煲部件、打印机色带导向器;适应SMT方式的连接器、插座、插件、插口、电源部件、开关、传感器、电容器座板、继电器、电阻器、熔断器支持件、线卷骨架、LC或 LED的外壳等为代表的电气/电子相关部件,汽车/车辆相关部件、家电/办公电器部件、计算机相关部件、传真机/复印机相关部件、机械相关部件及其它各种用途。
与现有技术相比,本发明的有益效果如下:
本发明通过将过量二羧酸单体与二胺单体进行聚合,随聚合反应进行到后期,反应体系中排出大部分水后,再通过加入高沸点二胺单体或低分子量富胺齐聚物来补齐物料配比,最终通过固相增粘或熔融缩聚反应即可得到高分子量半芳族聚酰胺;由于在主要排气过程中,二酸单体摩尔数过量,聚合体系中游离状态的二胺单体浓度低,大大降低了聚合过程中二胺单体的损失,具有良好的经济价值和环保价值。
具体实施方式
下面通过实施例的方式进一步说明本发明,但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法,按照常规方法和条件,或按照商品说明书选择。
实施例中用到的测试方法如下:
(1)聚酰胺树脂熔点:
聚酰胺树脂的熔点(Tm)通过差式扫描量热法DSC(Perkin Elmer Diamond)测定。样品的DSC测试中,Tm的结果来自于二次升温DSC曲线。DSC测试中,加热和冷却速率均为 10℃/min,测试过程中吹扫气和保护气均为氮气,吹扫气速率为20mL/min。熔点(Tm)选自二次升温曲线中熔融峰的峰值温度。
(2)特性粘度:
在25℃的浓硫酸中测量浓度为0.5、0.1、0.3和1g/dl的聚酰胺的对数比浓黏度ηinh。
ηinh=[ln(t1/t0)]/C
其中,ηinh表示对数比浓黏度(dl/g),t0表示溶剂的流过时间(sec),t1表示样品溶液的流过时间(sec),C表示样品溶液的浓度(g/dl)。
将ηinh的数据外推到浓度为0,以得到样品的特性黏度[η]。
(3)排出水中二元胺含量:
以甲基红为指示剂,采用标准浓度的稀盐酸溶液滴定所得,通过物料换算为二元胺的质量分数。
(4)力学性能,拉伸强度和断裂伸长率:
将制备的半芳香族聚酰胺注塑成型为哑铃形样条,根据ASTM的标准测试其拉伸强度和断裂伸长率。
实施例1:PA6T/66=50:50
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.046kg(9mol)己二胺、0.731kg(5mol)己二酸、0.831kg(5mol)对苯二甲酸、12.21g 苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。当反应体系中剩余水分含量为15%时,向反应体系中加入172.31g(1mol)癸二胺,继续搅拌反应。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过盘管冷却装置收集聚合过程中排出的水汽,通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
实施例2:PA6T/66=50:50
本实施例的聚合工艺条件与加料情况与实施例1相同,不同点仅在于将癸二胺改为 200.36g(1mol)的十二烷二胺。
实施例3:PA6T/66=50:50
本实施例的聚合工艺条件与加料情况与实施例1相同,不同点仅在于将癸二胺改为500g PA6T齐聚物;其中PA6T齐聚物采用摩尔比为3:2的己二胺与对苯二甲酸单体通过聚合所得,数均分子量500g/mol。
实施例4:PA6T/6I=65:35
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.046kg(9mol)己二胺、1.080kg(6.5mol)对苯二甲酸、0.581kg(3.5mol)间苯二甲酸、12.21g苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行 2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。当反应体系中剩余水分含量为15%时,向反应体系中加入172.31g(1mol)癸二胺,继续搅拌反应。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过盘管冷却装置收集聚合过程中排出的水汽,通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
实施例5:PA6T/6I/66=65:25:10
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.046kg(9mol)己二胺、1.080kg(6.5mol)对苯二甲酸、0.415kg(2.5mol)间苯二甲酸、0.146kg(1mol)己二酸、12.21g苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。当反应体系中剩余水分含量为15%时,向反应体系中加入172.31g(1mol)癸二胺,继续搅拌反应。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过盘管冷却装置收集聚合过程中排出的水汽,通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
实施例6:PA10T
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.551g(9mol)癸二胺、1.661kg(10mol)对苯二甲酸、12.21g苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。当反应体系中剩余水分含量为15%时,向反应体系中加入200.36g(1mol)十二烷二胺,继续搅拌反应。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在 250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过盘管冷却装置收集聚合过程中排出的水汽,通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
实施例1-6测试结果及物料配比见表1。
表1实施例1-6加料情况及实验结果
项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 |
己二胺/mol | 9 | 9 | 9 | 9 | 9 | - |
癸二胺/mol | - | - | - | - | - | 9 |
己二酸/mol | 5 | 5 | 5 | - | 1.0 | - |
对苯二甲酸/mol | 5 | 5 | 5 | 6.5 | 6.5 | 10 |
间苯二甲酸/mol | - | - | - | 3.5 | 2.5 | - |
癸二胺/mol | 1 | - | - | 1 | 1 | - |
十二烷二胺/mol | - | 1 | - | - | - | 1 |
富胺齐聚物/g | - | - | 500 | - | - | - |
苯甲酸/mol | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
次磷酸钠/g | 1 | 1 | 1 | 1 | 1 | 1 |
预聚物特性黏度(dl/g) | 0.162 | 0.163 | 0.172 | 0.165 | 0.174 | 0.166 |
半芳聚酰胺特性黏度(dl/g) | 1.55 | 1.53 | 1.58 | 1.56 | 1.51 | 1.54 |
半芳聚酰胺熔点/℃ | 305 | 302 | 310 | 301 | 308 | 313 |
排出水中二元胺含量/wt% | 0.06 | 0.05 | 0.07 | 0.05 | 0.06 | 0.05 |
实施例7:PA6T/66=50:50
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.046kg(9mol)己二胺、0.731kg(5mol)己二酸、0.831kg(5mol)对苯二甲酸、12.21g 苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,将所得预聚物与172.31g(1mol)癸二胺通过高速混合机混合,混合后的物料通过双螺杆挤出机熔融挤出增粘。挤出温度设定为320-330℃,停留时间控制在8分钟,反应过程中产生水汽通过挤出机的真空排气口除去,得到最终的半芳族聚酰胺树脂。
通过盘管冷却装置收集聚合釜聚合过程中排出的水汽,通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
实施例8:PA6T/66=50:50
本实施例的聚合工艺条件与加料情况与实施例7相同,不同点仅在于将癸二胺改为 200.36g(1mol)十二烷二胺。
实施例9:PA6T/66=50:50
本实施例的聚合工艺条件与加料情况与实施例7相同,不同点仅在于将癸二胺改为500g PA6T齐聚物;其中PA6T齐聚物采用摩尔比为3:2的己二胺与对苯二甲酸单体通过聚合所得,数均分子量500g/mol。
实施例7-9测试结果及物料配比见表2。
表2实施例7-9加料情况及实验结果
对比例1:PA6T/66=50:50
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.185kg(10.2mol)己二胺、0.731kg(5mol)己二酸、0.831kg(5mol)对苯二甲酸、12.21g 苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
对比例2:PA6T/6I=65:35
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.185kg(10.2mol)己二胺、1.080kg(6.5mol)对苯二甲酸、0.581kg(3.5mol)间苯二甲酸、12.21g苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行 2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
对比例3:PA6T/6I/66=65:25:10
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.185kg(10.2mol)己二胺、1.080kg(6.5mol)对苯二甲酸、0.415kg(2.5mol)间苯二甲酸、0.146kg(1mol)己二酸、12.21g苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在 220℃、2MPa条件下继续进行2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
对比例4:PA10T
10L不锈钢高压聚合反应釜,釜外装有加热夹套,釜内装有磁力密封的机械搅拌和测量釜内温度的热电偶,釜盖配有用于加料的加料口、进排气口、爆破片及压力表。向反应釜中加入1.758kg(10mol)癸二胺、1.661kg(10mol)对苯二甲酸、12.21g苯甲酸、1g次磷酸钠和3kg去离子水,物料加完后关闭加料阀,充排氮气三次,排出反应釜中空气。开启加热,当反应釜中温度达到95℃时,开启机械搅拌。在搅拌下继续升温至釜内温度上升至220℃。反应通过移去部分水而保持在220℃、2MPa条件下继续进行2小时。通过盘管冷却装置收集聚合过程中排出的水汽及二胺单体。反应结束后出料,从而得到预聚物。预聚物于80℃下真空干燥24小时,然后在250℃氮气气流下进行固相聚合10小时,得到最终的半芳族聚酰胺树脂。
通过稀盐酸溶液滴定可测定聚合过程中排出水汽中二元胺单体的含量,并通过换算,可计算出排出水汽中二元胺单体的质量分数。
对比例1-4测试结果及物料配比见表3。
表3对比例1-4加料情况及实验结果
项目 | 对比例1 | 对比例2 | 对比例3 | 对比例4 |
己二胺/mol | 10.2 | 10.2 | 10.2 | - |
癸二胺/mol | - | - | - | 10.2 |
己二酸/mol | 5 | - | 1.0 | - |
对苯二甲酸/mol | 5 | 6.5 | 6.5 | 10 |
间苯二甲酸/mol | - | 3.5 | 2.5 | - |
苯甲酸/mol | 0.1 | 0.1 | 0.1 | 0.1 |
次磷酸钠/g | 1 | 1 | 1 | 1 |
预聚物特性黏度(dl/g) | 0.158 | 0.165 | 0.181 | 0.167 |
半芳聚酰胺特性黏度(dl/g) | 1.51 | 1.56 | 1.58 | 1.61 |
半芳聚酰胺熔点/℃ | 306 | 301 | 309 | 314 |
排出水中二元胺含量/wt% | 1.50 | 1.43 | 1.62 | 0.98 |
从表1-3的结果来看,本发明通过聚合前期排水过程保证二酸单体过量,使游离二胺单体浓度降低,大幅减少了聚合排气过程中二胺单体组分的挥发。聚合后期,通过加入高沸点二胺单体或富胺齐聚物,保证了的酸胺单体摩尔量相近,从而得到了高分子量的芳香族聚酰胺树脂。
实施例10-13
将实施例1-4制备的半芳族聚酰胺树脂分别用于制备模塑组合物,其原料组成如表4所示。其中实施例10-13依次对应实施例1-4的半芳族聚酰胺树脂。
制备方法如下:
将实施例1-4所得半芳族聚酰胺树脂与配方量的抗氧剂、滑石粉通过V型转鼓混合均匀,再通过双螺杆挤出机挤出改性,其中配方量的玻璃纤维通过双螺杆挤出机侧喂料口加入,从而获得改性后的半芳族聚酰胺树脂。
将改性后的半芳族聚酰胺树脂通过注塑机注塑成型为哑铃形样条,根据ASTM的标准通过拉力机测试样条拉伸强度和断裂伸长率。测试结果如表4所示。
表4实施例10-13的组合物原料组成及力学测试结果
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Claims (8)
1.一种减少二胺单体损失的半芳族聚酰胺制备方法,其特征在于:包括以下步骤:
(1)以二元羧酸单体A和二元胺单体B为原料,在催化剂和封端剂的作用下,在水中进行聚合反应2~12h后,再加入高沸点二胺单体C和/或低分子量富胺齐聚物D,继续聚合反应,得到预聚物;
(2)将预聚物进行固相增粘或熔融缩聚反应,得到半芳族聚酰胺;
所述高沸点二胺单体C为癸二胺或十二烷二胺;
所述低分子量富胺齐聚物D为PA6T齐聚物,采用摩尔比为3:2的己二胺与对苯二甲酸单体通过聚合所得,数均分子量500g/mol;
二元羧酸单体A的摩尔总数为a,二元胺单体B摩尔总数为b,高沸点二胺单体C和/或低分子量富胺齐聚物D的摩尔总数为c,二元羧酸单体A和二元胺单体B的摩尔比为10:9,定义参数R=a/(b+c),R的取值为1。
2.根据权利要求1所述的减少二胺单体损失的半芳族聚酰胺制备方法,其特征在于:所述二元羧酸单体A为含有4~36个碳原子的二元羧酸单体,包括脂肪结构二羧酸单体、脂环结构二羧酸单体和/或芳香结构二羧酸单体,脂肪结构或脂环结构二元羧酸单体;
所述二元胺单体B为含有2~36个碳原子的二元胺单体,包括脂肪结构二元胺单体、脂环结构二元胺单体和/或芳香结构二元胺单体,脂肪结构或脂环结构二元胺单体。
3.根据权利要求1所述的减少二胺单体损失的半芳族聚酰胺制备方法,其特征在于:所述催化剂选自无机和/或有机磷、锡或铅化合物及其混合物;催化剂的用量为聚合单体总重量的0.0001~5wt%。
4.根据权利要求1所述的减少二胺单体损失的半芳族聚酰胺制备方法,其特征在于:封端剂选自脂肪结构单羧酸化合物、脂环结构单羧酸化合物、芳香结构单羧酸化合物、脂肪结构单胺化合物、脂环结构单胺化合物和芳族单胺化合物中的一种或多种;封端剂的用量为聚合单体总重量的0.01~10wt%。
5.根据权利要求1所述的减少二胺单体损失的半芳族聚酰胺制备方法,其特征在于:步骤(1)中,聚合反应的反应温度为200~300℃,反应压力为0.5~5MPa。
6.根据权利要求1所述的减少二胺单体损失的半芳族聚酰胺制备方法,其特征在于:步骤(2)中,固相增粘反应在惰性气体氛围或真空条件下进行,反应温度220~280℃,反应时间2~24小时;熔融缩聚在带有排气口的挤出设备中进行,反应温度280~350℃,反应时间在0.5小时以内。
7.一种半芳族聚酰胺,其特征在于:由权利要求1-6任一项所述的制备方法制备得到,其熔点为250-350℃。
8.一种权利要求7所述的半芳族聚酰胺组成的模塑组合物,其特征在于:包括以下重量份数的原料:
半芳族聚酰胺 30~100份,
增强材料 0~70份,
无机填料 0~70份,
添加剂 0~60份;
所述添加剂包括抗氧剂、阻燃剂、润滑剂、脱模剂、成核剂、着色剂、增塑剂、增韧剂、抗静电剂、增溶剂、分散剂、稳定剂、流动改性剂或其他聚合物树脂中的一种或多种。
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CN108559076A (zh) * | 2018-04-08 | 2018-09-21 | 金发科技股份有限公司 | 一种半芳香族聚酰胺树脂及其制备方法和由其组成的聚酰胺模塑组合物 |
CN111057233A (zh) * | 2019-12-29 | 2020-04-24 | 无锡殷达尼龙有限公司 | 一种共聚半芳香族聚酰胺及其制备方法 |
CN112592472A (zh) * | 2020-12-16 | 2021-04-02 | 浙江新和成特种材料有限公司 | 一种低聚物含量低的半芳香族聚酰胺连续化制备方法及其产品 |
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