CN107075378B - 阻燃剂组合物及阻燃性合成树脂组合物 - Google Patents
阻燃剂组合物及阻燃性合成树脂组合物 Download PDFInfo
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- CN107075378B CN107075378B CN201580062883.1A CN201580062883A CN107075378B CN 107075378 B CN107075378 B CN 107075378B CN 201580062883 A CN201580062883 A CN 201580062883A CN 107075378 B CN107075378 B CN 107075378B
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- C08K5/0066—Flame-proofing or flame-retarding additives
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- C08K13/02—Organic and inorganic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
本发明提供阻燃性和加工性优异的阻燃剂组合物,此外还提供配合了该阻燃剂组合物的阻燃性和加工性优异的阻燃性合成树脂组合物,具体而言,将20~50质量份的作为(A)成分的选自正磷酸三聚氰胺、焦磷酸三聚氰胺、多磷酸三聚氰胺的组中的一种以上的三聚氰胺盐、50~80质量份的作为(B)成分的选自正磷酸哌嗪、焦磷酸哌嗪、多磷酸哌嗪的组中的一种以上的哌嗪盐(其中(A)成分和(B)成分的合计为100质量份)、0.01~20.0质量份的作为(C)成分的下述通式(1)所表示的二环磷酸酯化合物并用。关于式(1)的详细情况如本说明书中记载的那样。
Description
技术领域
本发明涉及合成树脂用的阻燃剂组合物及配合了该阻燃剂组合物的阻燃性合成树脂组合物,涉及阻燃性和加工性优异的阻燃剂组合物及配合了该阻燃剂组合物的阻燃性合成树脂组合物。
背景技术
以往,合成树脂由于其优异的化学特性、机械特性而被广泛用于建筑材料、汽车部件、包装用材料、农业用材料、家电制品的外壳材料、玩具等中。可是,大多的合成树脂为可燃性物质,根据用途而阻燃化是不可或缺的。进而,作为阻燃化方法,众所周知是单独或组合使用卤素系阻燃剂、以红磷或聚磷酸铵(也可称为多聚磷酸铵)等聚磷酸系阻燃剂为代表的无机磷系阻燃剂、以三芳基磷酸酯化合物为代表的有机磷系阻燃剂、金属氢氧化物或作为阻燃助剂的氧化锑、三聚氰胺化合物。
例如在专利文献1中记载了:特别是以多磷酸或焦磷酸与含氮化合物的盐作为主要成分的、通过在燃烧时形成表面膨胀层(Intumescent)而抑制分解产物的扩散或传热来发挥阻燃性的膨胀系阻燃剂具有优异的阻燃性。
此外,在专利文献2中,还提出了将三聚氰胺磷酸盐、聚磷酸铵等氮化合物与二环式磷酸酯化合物并用的阻燃剂。
然而,这些以往的阻燃剂存在阻燃性不充分、为了对合成树脂赋予充分的阻燃性需要大量的添加的问题。此外若大量添加、或原本阻燃剂相对于合成树脂的分散性差,则具有加工时间变长,或者需要高的加工温度或提高加工机的螺杆转速等,由此树脂被加热至必要温度以上而导致产生发泡等成形不良等加工性的问题,需要阻燃性和加工性优异的阻燃剂。
现有技术文献
专利文献
专利文献1:美国专利公开2003/0088000号公报
专利文献2:美国专利4341694号公报
发明内容
发明所要解决的问题
因此,本发明的目的在于提供阻燃性和加工性优异的阻燃剂组合物。此外还在于提供配合了该阻燃剂组合物的阻燃性和加工性优异的阻燃性合成树脂组合物。
用于解决问题的手段
本发明人们为了解决上述课题进行了深入研究,结果完成了本发明。
即,本发明提供一种阻燃剂组合物,其含有20~50质量份的下述(A)成分、50~80质量份的下述(B)成分(其中(A)成分和(B)成分的合计为100质量份)、0.01~20.0质量份的下述(C)成分。
(A)成分:选自正磷酸三聚氰胺、焦磷酸三聚氰胺、多磷酸三聚氰胺的组中的一种以上的三聚氰胺盐
(B)成分:选自正磷酸哌嗪、焦磷酸哌嗪、多磷酸哌嗪的组中的一种以上的哌嗪盐
(C)成分:下述通式(1)所表示的二环磷酸酯化合物
(式(1)中,R表示碳原子数为1~4的烷基、或碳原子数为1~4的羟基烷基。)
此外本发明提供上述阻燃剂组合物,其中,进一步含有0.01~10质量份的氧化锌作为(D)成分。
此外本发明提供一种阻燃性合成树脂组合物,其在合成树脂中配合了上述阻燃剂组合物。
此外本发明提供上述阻燃性合成树脂组合物,其中,合成树脂为聚烯烃系树脂。
此外本发明提供一种成形体,其是由上述阻燃性合成树脂组合物得到的。
发明效果
根据本发明,能够提供阻燃性和加工性优异的阻燃剂组合物。此外根据本发明,能够提供阻燃性和加工性优异的阻燃性合成树脂组合物。此外根据本发明,能够提供具有优异的阻燃性的成形体。
具体实施方式
基于优选的实施方式,对本发明的阻燃剂组合物进行详细说明。
本发明的阻燃剂组合物中作为(A)成分使用的三聚氰胺盐选自正磷酸三聚氰胺、焦磷酸三聚氰胺、多磷酸三聚氰胺的组中,它们可以单独使用也可以以混合物使用。它们中,从阻燃性、处理性、保存稳定性的方面出发,优选焦磷酸三聚氰胺。将它们以混合物使用的情况下,焦磷酸三聚氰胺的含有比例优选较高。此外焦磷酸三聚氰胺的焦磷酸与三聚氰胺的比以摩尔比计优选为1:2。
这些磷酸与三聚氰胺的盐也可以通过使分别对应的磷酸或磷酸盐与三聚氰胺反应来得到,但本发明的(A)成分中使用的三聚氰胺盐优选使正磷酸1三聚氰胺加热缩合而得到的焦磷酸三聚氰胺或多磷酸三聚氰胺,特别优选焦磷酸三聚氰胺。
本发明的阻燃剂组合物中作为(B)成分使用的哌嗪盐选自正磷酸哌嗪、焦磷酸哌嗪、多磷酸哌嗪的组中,它们可以单独使用也可以以混合物使用。它们中,从阻燃性、处理性、保存稳定性的方面出发,优选焦磷酸哌嗪,在以混合物使用的情况下,焦磷酸哌嗪的含有比例越高越优选。此外焦磷酸哌嗪的焦磷酸与哌嗪的比以摩尔比计优选为1:1。
这些磷酸与哌嗪的盐也可以通过使分别对应的磷酸或磷酸盐与哌嗪反应来得到,但本发明的(B)成分中使用的哌嗪盐优选使2正磷酸1哌嗪加热缩合而得到的焦磷酸哌嗪或多磷酸哌嗪,特别优选焦磷酸哌嗪。
关于本发明的阻燃剂组合物中的(A)成分和(B)成分的含量,设(A)成分和(B)成分的合计为100质量份,(A)成分为20~50质量份、(B)成分为50~80质量份,优选(A)成分为30~45质量份、(B)成分为55~70质量份。
接着,对本发明的阻燃剂组合物的(C)成分进行说明。
本发明的阻燃剂组合物中的(C)成分为下述通式(1)所表示的二环磷酸酯化合物。
(式(1)中,R表示碳原子数为1~4的烷基或碳原子数为1~4的羟基烷基。)
在上述通式(1)中的R中,作为碳原子数为1~4的烷基,可以是直链的烷基,也可以是支链的烷基,可列举出例如甲基、乙基、丙基、异丙基、丁基、异丁基、仲丁基、叔丁基等,作为碳原子数为1~4的羟基烷基,可列举出将上述碳原子数为1~4的烷基的一个氢原子以羟基取代而得到的基团,可列举出例如羟基甲基、羟基乙基、羟基丙基、羟基丁基等。
作为R,从阻燃性和合成树脂的加工性的方面出发,优选羟基甲基。
作为本发明的上述通式(1)所表示的二环磷酸酯化合物,可列举出例如下述的化合物No.1~No.6等化合物,从阻燃性和合成树脂的加工性的方面出发,优选化合物No.1。
化合物No.1
化合物No.2
化合物No.3
化合物No.4
化合物No.5
化合物No.6
本发明的上述通式(1)所表示的二环磷酸酯化合物可以通过以往公知的方法来制造。作为这样的方法,可列举出例如美国专利第3293327号公报中公开的方法等。
本发明的阻燃剂组合物中的(C)成分即二环磷酸酯化合物的含量相对于(A)成分和(B)成分的合计100质量份为0.01~20.0质量份,从阻燃性、合成树脂的加工性的方面出发,优选为0.1~10.0质量份,更优选为1.0~8.0质量份,进一步更优选为3.0~8.0质量份。若低于0.01质量份,则得不到充分的阻燃性和加工性,若超过20.0质量份,则对树脂物性造成不良影响。
本发明的阻燃剂组合物优选进一步含有阻燃助剂即氧化锌作为(D)成分。该氧化锌也可以进行过表面处理。氧化锌可以使用市售品,可列举出例如氧化锌1种(三井金属矿业株式会社制)、部分覆膜型氧化锌(三井金属矿业株式会社制)、Nanofine 50(平均粒径为0.02μm的超微粒子氧化锌:堺化学工业株式会社制)、Nanofine K(平均粒径为0.02μm的硅酸锌覆膜的超微粒子氧化锌:堺化学工业株式会社制)等。
本发明的阻燃剂组合物中的(D)成分即氧化锌的含量从阻燃性的方面出发,相对于(A)成分和(B)成分的合计100质量份优选为0.01~10质量份,更优选为0.5~10质量份,进一步更优选为1.0~7.5质量份。
从防止阻燃剂粉末凝聚、保存稳定性提高和在合成树脂中的分散性提高的方面出发,本发明的阻燃剂组合物还可以含有硅油。
作为硅油的例子,可列举出聚硅氧烷的侧链、末端全部为甲基的二甲基硅油;聚硅氧烷的侧链、末端为甲基、且该侧链的一部分为苯基的甲基苯基硅油;聚硅氧烷的侧链、末端为甲基、且该侧链的一部分为氢的甲基氢硅油等、或它们的共聚物,此外也可以使用在它们的侧链和/或末端的一部分上导入了有机基团的氨基改性、环氧基改性、脂环式环氧基改性、羧基改性、甲醇改性、巯基改性、聚醚改性、长链烷基改性、氟代烷基改性、高级脂肪酸酯改性、高级脂肪酸酰胺改性、硅烷醇改性、二醇改性、酚改性和/或芳烷基改性而得到的改性硅油。
若列举出上述硅油的具体例子,则作为二甲基硅油,可列举出KF-96(信越化学株式会社制)、KF-965(信越化学株式会社制)、KF-968(信越化学株式会社制)等,作为甲基氢硅油,可列举出KF-99(信越化学株式会社制)、KF-9901(信越化学株式会社)、HMS-151(Gelest社制)、HMS-071(Gelest社制)、HMS-301(Gelest社制)、DMS-H21(Gelest社制)等,作为甲基苯基硅油的例子,可列举出KF-50(信越化学株式会社制)、KF-53(信越化学株式会社制)、KF-54(信越化学株式会社制)、KF-56(信越化学株式会社制)等,作为环氧基改性品,可列举出例如X-22-343(信越化学株式会社制)、X-22-2000(信越化学株式会社制)、KF-101(信越化学株式会社制)、KF-102(信越化学株式会社制)、KF-1001(信越化学株式会社制),作为羧基改性品,可列举出例如X-22-3701E(信越化学株式会社制),作为甲醇改性品,可列举出例如X-22-4039(信越化学株式会社制)、X-22-4015(信越化学株式会社制),作为氨基改性品,可列举出例如KF-393(信越化学株式会社制)等。
在本发明的阻燃剂组合物中,硅油中,从防止阻燃剂粉末凝聚、保存稳定性的提高和在合成树脂中的分散性提高的方面出发,优选为甲基氢硅油。
关于使本发明的阻燃剂组合物中含有硅油时的含量,从阻燃性、防止阻燃剂粉末凝聚、保存稳定性的提高和在合成树脂中的分散性提高的方面出发,相对于(A)成分和(B)成分的合计100质量份优选为0.01~5.0质量份,更优选为0.05~3.0质量份,进一步更优选为0.1~2.0质量份。
此外,为了防止阻燃剂粉末的凝聚、保存稳定性的提高、或为了赋予耐水性、耐热性,本发明的阻燃剂组合物还可以含有硅烷偶联剂。
作为硅烷偶联剂,例如作为具有链烯基的硅烷偶联剂,可列举出乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三乙酰氧基硅烷、乙烯基三(2-甲氧基乙氧基)硅烷、乙烯基甲基二甲氧基硅烷、辛烯基三甲氧基硅烷、烯丙基三甲氧基硅烷、对苯乙烯基三甲氧基硅烷等,作为具有丙烯酸基的硅烷偶联剂,可列举出3-丙烯酰氧基丙基三甲氧基硅烷、3-丙烯酰氧基丙基三乙氧基硅烷等,作为具有甲基丙烯酸基的硅烷偶联剂,可列举出3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二乙氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、甲基丙烯酰氧基辛基三甲氧基硅烷等,作为具有环氧基的硅烷偶联剂,可列举出2-(3,4-环氧环己基)乙基三甲氧基硅烷、3-环氧丙氧基丙基甲基二甲氧基硅烷、3-环氧丙氧基丙基三甲氧基硅烷、3-环氧丙氧基丙基甲基二乙氧基硅烷、3-环氧丙氧基丙基三乙氧基硅烷、环氧丙氧基辛基三甲氧基硅烷等,作为具有氨基的硅烷偶联剂,可列举出N-2-(氨基乙基)-3-氨基丙基甲基二甲氧基硅烷、N-2-(氨基乙基)-3-氨基丙基三甲氧基硅烷、3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、3-三乙氧基甲硅烷基-N-(1,3-二甲基-亚丁基)丙基胺、N-苯基-3-氨基丙基三甲氧基硅烷、N,N’-双[3-(三甲氧基甲硅烷基)丙基]乙二胺、N-(乙烯基苄基)-2-氨基乙基-3-氨基丙基三甲氧基硅烷的盐酸盐等,作为具有异氰脲酸酯基的硅烷偶联剂,可列举出三-(三甲氧基甲硅烷基丙基)异氰脲酸酯,作为具有巯基的硅烷偶联剂,可列举出3-巯基丙基甲基二甲氧基硅烷、3-巯基丙基三甲氧基硅烷、3-巯基丙基三乙氧基硅烷等,作为具有脲基的硅烷偶联剂,可列举出3-脲基丙基三甲氧基硅烷、3-脲基丙基三乙氧基硅烷等,作为具有硫醚基的硅烷偶联剂,可列举出双(三乙氧基甲硅烷基丙基)四硫醚,作为具有硫代酯基的硅烷偶联剂,可列举出3-辛酰基硫-1-丙基三乙氧基硅烷,作为具有异氰酸酯基的硅烷偶联剂,可列举出3-异氰酸酯丙基三乙氧基硅烷、3-异氰酸酯丙基三甲氧基硅烷等。
这些硅烷偶联剂中,从防止阻燃剂粉末的凝聚、保存稳定性的提高、或耐水性、耐热性的方面出发,优选具有环氧基的硅烷偶联剂。
上述硅烷偶联剂可以使用市售品,若列举出其例子,则作为乙烯基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-1003、Momentive Performance MaterialsJapan公司制的A-171、Dow Corning Toray株式会社制的Z-6300、Wacker AsahikaseiSilicone株式会社制的GENIOSIL XL10、日美商事株式会社制的Sila-Ace S210等,作为乙烯基三乙氧基硅烷,可列举出信越化学工业株式会社制的KBE-1003、MomentivePerformance Materials Japan公司制的A-151、Dow Corning Toray株式会社制的Z-6519、Wacker Asahikasei Silicone株式会社制的GENIOSIL GF56、日美商事株式会社制的Sila-Ace S220等,作为乙烯基三乙酰氧基硅烷,可列举出Wacker Asahikasei Silicone株式会社制的GENIOSIL GF62,作为乙烯基三(2-甲氧基乙氧基)硅烷,可列举出MomentivePerformance Materials Japan公司制的A-172,作为乙烯基甲基二甲氧基硅烷,可列举出Momentive Performance Materials Japan公司制的A-2171、Wacker AsahikaseiSilicone株式会社制的GENIOSIL XL12等,作为辛烯基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-1083,作为烯丙基三甲氧基硅烷,可列举出Dow Corning Toray株式会社制的Z-6825,作为对苯乙烯基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-1403,作为3-丙烯酰氧基丙基三甲氧基硅烷,可列举出KBM-5103,作为3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-502、Dow Corning Toray株式会社制的Z-6033等,作为3-甲基丙烯酰氧基丙基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-503、Momentive Performance Materials Japan公司制的A-174、DowCorning Toray株式会社制的Z-6030、Wacker Asahikasei Silicone株式会社制的GENIOSIL GF31、日美商事株式会社制的Sila-Ace S710等,作为3-甲基丙烯酰氧基丙基甲基二乙氧基硅烷,可列举出信越化学工业株式会社制的KBE-502,作为3-甲基丙烯酰氧基丙基三乙氧基硅烷,可列举出信越化学工业株式会社制的KBE-503、Momentive PerformanceMaterials Japan公司制的Y-9936,作为甲基丙烯酰氧基辛基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-5803,作为2-(3,4-环氧环己基)乙基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-303、Momentive Performance Materials Japan公司制的A-186、Dow Corning Toray株式会社制的Z-6043、日美商事株式会社制的Sila-Ace S530等,作为3-环氧丙氧基丙基甲基二甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-402、Dow Corning Toray株式会社制的Z-6044、日美商事株式会社制的Sila-Ace S520等,作为3-环氧丙氧基丙基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-403、Momentive Performance Materials Japan公司制的A-187、Dow Corning Toray株式会社制的Z-6040、Wacker Asahikasei Silicone株式会社制的GENIOSIL GF80、日美商事株式会社制的Sila-Ace S510等,作为3-环氧丙氧基丙基甲基二乙氧基硅烷,可列举出信越化学工业株式会社制的KBE-402,作为3-环氧丙氧基丙基三乙氧基硅烷,可列举出信越化学工业株式会社制的KBE-403、Momentive Performance Materials Japan公司制的A-1871、WackerAsahikasei Silicone株式会社制的GENIOSIL GF82等,作为环氧丙氧基辛基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-4803,作为N-2-(氨基乙基)-3-氨基丙基甲基二甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-602、Momentive PerformanceMaterials Japan公司制的A-2120、Wacker Asahikasei Silicone株式会社制的GENIOSILGF-95、日美商事株式会社制的Sila-Ace S310等,作为N-2-(氨基乙基)-3-氨基丙基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-603、Momentive PerformanceMaterials Japan公司制的A-1120、Momentive Performance Materials Japan公司制的A-1122、Dow Corning Toray株式会社制的Z-6020、Dow Corning Toray株式会社制的Z-6094、Wacker Asahikasei Silicone株式会社制的GENIOSIL GF-91、日美商事株式会社制的Sila-Ace S320等,作为3-氨基丙基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-903、Momentive Performance Materials Japan公司制的A-1110、Dow Corning Toray株式会社制的Z-6610、日美商事株式会社制的Sila-Ace S360等,作为3-氨基丙基三乙氧基硅烷,可列举出KBE-903、Momentive Performance Materials Japan公司制的A-1100、DowCorning Toray株式会社制的Z-6011、日美商事株式会社制的Sila-Ace S330等,作为3-三乙氧基甲硅烷基-N-(1,3-二甲基-亚丁基)丙基胺,可列举出KBE-9103、日美商事株式会社制的Sila-Ace S340等,作为N-苯基-3-氨基丙基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-573、Momentive Performance Materials Japan公司制的Y-9669、DowCorning Toray株式会社制的Z-6883等,作为N,N’-双[3-(三甲氧基甲硅烷基)丙基]乙二胺,可列举出日美商事株式会社制的Sila-Ace XS1003,作为N-(乙烯基苄基)-2-氨基乙基-3-氨基丙基三甲氧基硅烷的盐酸盐,可列举出信越化学工业株式会社制的KBM-575、DowCorning Toray株式会社制的Z-6032、日美商事株式会社制的Sila-Ace S350等,作为三-(三甲氧基甲硅烷基丙基)异氰脲酸酯,可列举出信越化学工业株式会社制的KBM-9659,作为3-巯基丙基甲基二甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-802、DowCorning Toray株式会社制的Z-6852,作为3-巯基丙基三甲氧基硅烷,可列举出信越化学工业株式会社制的KBM-803、Momentive Performance Materials Japan公司制的A-189、DowCorning Toray株式会社制的Z-6062、日美商事株式会社制的Sila-Ace S810等,作为3-巯基丙基三乙氧基硅烷,可列举出Momentive Performance Materials Japan公司制的A-1891、Dow Corning Toray株式会社制的Z-6911,作为3-脲基丙基三乙氧基硅烷,可列举出Momentive Performance Materials Japan公司制的A-1160,作为3-脲基丙基三烷氧基硅烷,可列举出信越化学工业株式会社制的KBE-585,作为双(三乙氧基甲硅烷基丙基)四硫醚,可列举出信越化学工业株式会社制的KBE-846,作为3-辛酰基硫-1-丙基三乙氧基硅烷,可列举出Momentive Performance Materials Japan公司制的A-LINK599,作为3-异氰酸酯丙基三乙氧基硅烷,可列举出信越化学工业株式会社制的KBE-9007、MomentivePerformance Materials Japan公司制的A-1310等,作为3-异氰酸酯丙基三甲氧基硅烷,可列举出Momentive Performance Materials Japan公司制的Y-5187、Wacker AsahikaseiSilicone株式会社制的GENIOSIL GF40等。
在本发明的阻燃剂组合物中配合硅烷偶联剂时的其含量相对于(A)成分和(B)成分的合计100质量份优选为0.01~5.0质量份,更优选为0.05~3.0质量份,进一步更优选为0.1~2.0质量份。
此外本发明的阻燃剂组合物在不损害本发明的效果的范围内,根据需要还可以配合防滴落剂。作为防滴落剂,可列举出氟系防滴落剂或硅橡胶类、层状硅酸盐等。
作为上述层状硅酸盐,可列举出蒙脱石、皂石、锂蒙脱石、贝得石、硅镁石、绿脱石等蒙脱石系粘土矿物、蛭石、埃洛石、溶胀性云母、滑石等,在其层间还可以插入有机阳离子、季铵阳离子、鏻阳离子。
上述防滴落剂特别优选氟系的防滴落剂,作为氟系的防滴落剂的具体例子,可列举出例如聚四氟乙烯、聚偏氟乙烯、聚六氟丙烯等氟系树脂或全氟甲磺酸钠盐、全氟正丁烷磺酸钾盐、全氟叔丁烷磺酸钾盐、全氟辛烷磺酸钠盐、全氟-2-乙基己烷磺酸钙盐等全氟链烷烃磺酸碱金属盐化合物或全氟链烷烃磺酸碱土类金属盐等。防滴落剂中,从防滴落性的方面出发,最优选聚四氟乙烯。
含有上述防滴落剂时的防滴落剂的含量相对于(A)成分和(B)成分的合计100质量份优选为0.005~5质量份,更优选为0.01~5质量份,进一步优选为0.05~3质量份,最优选为0.1~1质量份。若低于0.005质量份,则防滴落效果不充分,若超过5质量份,则有时使树脂的特性降低。
此外,在本发明的阻燃剂组合物中,在不损害本发明的效果的范围内,根据需要还可以配合多元醇化合物作为阻燃性助剂。多元醇化合物为键合有多个羟基的化合物,例如为季戊四醇、二季戊四醇、三季戊四醇、聚季戊四醇、新戊二醇、三羟甲基丙烷、二(三羟甲基)丙烷、1,3,5-三(2-羟乙基)异氰脲酸酯(THEIC)、聚乙二醇、甘油、二甘油、甘露糖醇、麦芽糖醇、乳糖醇、山梨糖醇、赤藓醇、木糖醇、木糖、蔗糖、海藻糖、肌醇、果糖、麦芽糖、乳糖等。这些多元醇化合物中,优选选自季戊四醇、二季戊四醇、三季戊四醇、聚季戊四醇等季戊四醇、季戊四醇的缩合物的组中的一种以上,特别优选二季戊四醇、季戊四醇的缩合物,最优选二季戊四醇。此外,也可以适当使用THEIC及山梨糖醇。
含有上述多元醇化合物时的含量相对于(A)成分和(B)成分的合计100质量份优选为0.5~15质量份,更优选为2~12质量份,进一步优选为5~10质量份。
此外,在本发明的阻燃剂组合物中,在不损害本发明的效果的范围内,根据需要还可以配合润滑剂。作为这样的润滑剂,可列举出液体石蜡、天然石蜡、微晶石蜡、合成石蜡、低分子量聚乙烯、聚乙烯蜡等纯烃系润滑剂;卤代烃系润滑剂;高级脂肪酸、羟基脂肪酸等脂肪酸系润滑剂;脂肪酸酰胺、双脂肪酸酰胺等脂肪酸酰胺系润滑剂;脂肪酸的低级醇酯、甘油酯等脂肪酸的多元醇酯、脂肪酸的聚二醇酯、脂肪酸的脂肪醇酯(酯蜡)等酯系润滑剂;金属皂、脂肪醇、多元醇、聚二醇、聚甘油、脂肪酸与多元醇的部分酯、脂肪酸与聚二醇、聚甘油的部分酯系的润滑剂、硅油、矿物油等。润滑剂也可以是两种以上。含有润滑剂时的含量相对于(A)成分和(B)成分的合计100质量份优选为0.05~10质量份,更优选为0.1~5质量份。
从耐热性、降低加工机的腐蚀风险、耐候性的方面出发,本发明的阻燃剂组合物还可以进一步含有水滑石化合物。本发明中,水滑石化合物是指镁和/或锌与铝的碳酸复盐化合物。水滑石系化合物可以是天然物,此外也可以是合成品。作为合成品的合成方法,可例示出日本特公昭46-2280号公报、日本特公昭50-30039号公报、日本特公昭51-29129号公报、日本特开昭61-174270号公报等中记载的公知的方法。此外,本发明中,对于水滑石系化合物的晶体结构、晶体粒径或者结晶水的有无及其量等可以没有限制地使用。
此外水滑石化合物也可以进行高氯酸处理,还可以将其表面以硬脂酸那样的高级脂肪酸、油酸碱金属盐那样的高级脂肪酸金属盐、十二烷基苯磺酸碱金属盐那样的有机磺酸金属盐、高级脂肪酸酰胺、高级脂肪酸酯或蜡等被覆后使用。
作为水滑石化合物,可以使用下述通式(4)所表示的化合物。
Mgx1Znx2Al2(OH)2(X1+X2)+4·CO3·mH2O (4)
(式中,x1及x2各自表示满足下述式所表示的条件的数,m表示实数。0≤x2/x1<10、2≤x1+x2<20)
此外作为水滑石化合物,也可以使用包含锌的锌改性水滑石。
上述水滑石系化合物可以使用市售品,可列举出例如DHT-4(水滑石:协和化学工业株式会社制)、DHT-4A(水滑石:协和化学工业株式会社制)、Magceler-1(水滑石:协和化学工业株式会社制)、Alcamizer-1(水滑石:协和化学工业株式会社制)、Alcamizer-2(水滑石:协和化学工业株式会社制)、Alcamizer-4(Alcamizer-P-93)(锌改性水滑石:协和化学工业株式会社制)、Alcamizer-7(锌改性水滑石:协和化学工业株式会社制)、Alcamizer-5(高氯酸处理水滑石:协和化学工业株式会社制)等,特别优选DHT-4A(水滑石:协和化学工业株式会社制)。
本发明的阻燃剂组合物中的水滑石化合物的含量相对于(A)成分和(B)成分的合计100质量份优选为0.01~5质量份,从耐热性、降低加工机的腐蚀风险、耐候性的方面出发,更优选为0.05~4质量份,进一步更优选为0.1~2质量份。
在本发明的阻燃剂组合物中,在不损害本发明的效果的范围内,根据需要还可以使用不含有卤素的有机或无机系的阻燃剂或阻燃助剂中的一种以上。作为这些阻燃剂·阻燃助剂,可列举出含三嗪环的化合物、金属氢氧化物、磷酸酯系阻燃剂、缩合磷酸酯系阻燃剂、磷酸盐系阻燃剂、无机磷系阻燃剂、二烷基次膦酸盐、硅酮系阻燃剂、金属氧化物、硼酸化合物、膨胀性石墨、其他无机系阻燃助剂、其他有机系阻燃剂等。
作为上述含三嗪环的化合物,可列举出例如三聚氰胺、三聚氰酸二酰胺、苯并胍胺、乙酰胍胺、邻苯二胍胺(phthalodiguanamine)、三聚氰胺氰脲酸酯、亚丁基二胍胺、降冰片烯二胍胺、亚甲基二胍胺、亚乙基双三聚氰胺、三亚甲基双三聚氰胺、四亚甲基双三聚氰胺、六亚甲基双三聚氰胺、1,3-亚己基双三聚氰胺等。
作为上述金属氢氧化物,可列举出氢氧化镁、氢氧化铝、氢氧化钙、氢氧化钡、氢氧化锌、KISUMA 5A(协和化学工业株式会社制氢氧化镁的商标)等。
作为上述磷酸酯系阻燃剂的例子,可列举出例如磷酸三甲酯、磷酸三乙酯、磷酸三丁酯、磷酸三(丁氧基乙基)酯、磷酸三(氯乙基)酯、磷酸三(二氯丙基)酯、磷酸三苯酯、磷酸三甲苯酯、磷酸甲苯基二苯基酯、磷酸三(二甲苯基)酯、磷酸辛基二苯基酯、磷酸二甲苯基二苯基酯、磷酸三异丙基苯基酯、磷酸2-乙基己基二苯基酯、磷酸叔丁基苯基二苯基酯、双-(叔丁基苯基)苯基磷酸酯、三-(叔丁基苯基)磷酸酯、磷酸异丙基苯基二苯基酯、双-(异丙基苯基)二苯基磷酸酯、三-(异丙基苯基)磷酸酯等。
作为上述缩合磷酸酯系阻燃剂的例子,可列举出1,3-亚苯基双(二苯基磷酸酯)、1,3-亚苯基双(双二甲苯基磷酸酯)、双酚A双(二苯基磷酸酯)等。
作为上述无机磷系阻燃剂,可列举出红磷。
作为上述二烷基次膦酸盐,可列举出二乙基次膦酸铝、二乙基次膦酸锌等。
作为上述其他无机系阻燃助剂,可列举出例如氧化钛、氧化铝、氧化镁、水滑石等无机化合物、及其表面处理品。作为其具体例子,可以使用例如TIPAQUE R-680(石原产业株式会社制氧化钛的商标)、Kyowa Mag150(协和化学工业株式会社制氧化镁的商标)、DHT-4A(水滑石:协和化学工业株式会社制)、Alcamizer-4(协和化学工业株式会社制锌改性水滑石的商标)等各种市售品。
本发明中使用的阻燃剂组合物根据需要还可以配合酚系抗氧化剂、磷系抗氧化剂、硫醚系抗氧化剂、紫外线吸收剂、受阻胺系光稳定剂、防老化剂等。这些成分可以预先配合到本发明的阻燃剂组合物中,也可以在配合到合成树脂中时配合到合成树脂中。优选通过配合它们而使合成树脂稳定化。
作为上述酚系抗氧化剂,可列举出例如2,6-二叔丁基-对甲酚、2,6-二苯基-4-十八烷氧基苯酚、二硬脂基(3,5-二叔丁基-4-羟基苄基)膦酸酯、1,6-六亚甲基双〔(3,5-二叔丁基-4-羟基苯基)丙酸酰胺〕、4,4'-硫代双(6-叔丁基-间甲酚)、2,2'-亚甲基双(4-甲基-6-叔丁基苯酚)、2,2'-亚甲基双(4-乙基-6-叔丁基苯酚)、4,4'-亚丁基双(6-叔丁基-间甲酚)、2,2'-亚乙基双(4,6-二叔丁基苯酚)、2,2'-亚乙基双(4-仲丁基-6-叔丁基苯酚)、1,1,3-三(2-甲基-4-羟基-5-叔丁基苯基)丁烷、1,3,5-三(2,6-二甲基-3-羟基-4-叔丁基苄基)异氰脲酸酯、1,3,5-三(3,5-二叔丁基-4-羟基苄基)异氰脲酸酯、1,3,5-三(3,5-二叔丁基-4-羟基苄基)-2,4,6-三甲基苯、2-叔丁基-4-甲基-6-(2-丙烯酰氧基-3-叔丁基-5-甲基苄基)苯酚、硬脂基(3,5-二叔丁基-4-羟基苯基)丙酸酯、四〔3-(3,5-二叔丁基-4-羟基苯基)丙酸甲基〕甲烷、硫代二乙二醇双〔(3,5-二叔丁基-4-羟基苯基)丙酸酯〕、1,6-六亚甲基双〔(3,5-二叔丁基-4-羟基苯基)丙酸酯〕、双〔3,3-双(4-羟基-3-叔丁基苯基)丁酸〕二醇酯、双〔2-叔丁基-4-甲基-6-(2-羟基-3-叔丁基-5-甲基苄基)苯基〕对苯二甲酸酯、1,3,5-三〔(3,5-二叔丁基-4-羟基苯基)丙酰氧基乙基〕异氰脲酸酯、3,9-双〔1,1-二甲基-2-{(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基}乙基〕-2,4,8,10-四氧杂螺〔5,5〕十一烷、三乙二醇双〔(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯〕等。
这些酚系抗氧化剂的使用量在配合到合成树脂中时,在合成树脂组合物中优选为0.001~5质量%,更优选为0.05~3质量%。
作为上述磷系抗氧化剂,可列举出例如亚磷酸三(壬基苯基)酯、三〔2-叔丁基-4-(3-叔丁基-4-羟基-5-甲基苯基硫基)-5-甲基苯基〕亚磷酸酯、亚磷酸十三烷基酯、辛基二苯基亚磷酸酯、二(癸基)单苯基亚磷酸酯、二(十三烷基)季戊四醇二亚磷酸酯、二(壬基苯基)季戊四醇二亚磷酸酯、双(2,4-二叔丁基苯基)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(2,4,6-三叔丁基苯基)季戊四醇二亚磷酸酯、双(2,4-二枯基苯基)季戊四醇二亚磷酸酯、四(十三烷基)异亚丙基二苯酚二亚磷酸酯、四(十三烷基)-4,4'-正亚丁基双(2-叔丁基-5-甲基苯酚)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、四(2,4-二叔丁基苯基)联亚苯基二亚膦酸酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、2,2'-亚甲基双(4,6-叔丁基苯基)-2-乙基己基亚磷酸酯、2,2'-亚甲基双(4,6-叔丁基苯基)-十八烷基亚磷酸酯、2,2'-亚乙基双(4,6-二叔丁基苯基)氟代亚磷酸酯、三(2-〔(2,4,8,10-四叔丁基二苯并〔d,f〕〔1,3,2〕二噁磷杂庚英-6-基)氧〕乙基)胺、2-乙基-2-丁基丙二醇与2,4,6-三叔丁基苯酚的亚磷酸酯等。这些磷系抗氧化剂的使用量在配合到合成树脂中时,在合成树脂组合物中优选为0.001~5质量%,更优选为0.05~3质量%。
作为上述硫醚系抗氧化剂,可列举出例如硫代二丙酸二月桂酯、硫代二丙酸二肉豆蔻酯、硫代二丙酸二硬脂酯等硫代二丙酸二烷基酯类、及季戊四醇四(β-烷基硫代丙酸)酯类。这些硫醚系抗氧化剂的使用量在配合到合成树脂中时,在合成树脂组合物中优选为0.001~5质量%,更优选为0.05~3质量%。
作为上述紫外线吸收剂,可列举出例如2,4-二羟基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-羟基-4-辛氧基二苯甲酮、5,5'-亚甲基双(2-羟基-4-甲氧基二苯甲酮)等2-羟基二苯甲酮类;2-(2'-羟基-5'-甲基苯基)苯并三唑、2-(2'-羟基-3',5'-二叔丁基苯基)-5-氯苯并三唑、2-(2'-羟基-3'-叔丁基-5'-甲基苯基)-5-氯苯并三唑、2-(2'-羟基-5'-叔辛基苯基)苯并三唑、2-(2'-羟基-3',5'-二枯基苯基)苯并三唑、2,2'-亚甲基双(4-叔辛基-6-(苯并三唑基)苯酚)、2-(2'-羟基-3'-叔丁基-5'-羧基苯基)苯并三唑等2-(2'-羟基苯基)苯并三唑类;水杨酸苯酯、间苯二酚单苯甲酸酯、2,4-二叔丁基苯基-3,5-二叔丁基-4-羟基苯甲酸酯、2,4-二叔戊基苯基-3,5-二叔丁基-4-羟基苯甲酸酯、十六烷基-3,5-二叔丁基-4-羟基苯甲酸酯等苯甲酸酯类;2-乙基-2'-乙氧基草酰替苯胺、2-乙氧基-4'-十二烷基草酰替苯胺等取代草酰替苯胺类;乙基-α-氰基-β、β-二苯基丙烯酸酯、甲基-2-氰基-3-甲基-3-(对甲氧基苯基)丙烯酸酯等氰基丙烯酸酯类;2-(2-羟基-4-辛氧基苯基)-4,6-双(2,4-二叔丁基苯基)-s-三嗪、2-(2-羟基-4-甲氧基苯基)-4,6-二苯基-s-三嗪、2-(2-羟基-4-丙氧基-5-甲基苯基)-4,6-双(2,4-二叔丁基苯基)-s-三嗪等三芳基三嗪类。这些紫外线吸收剂的使用量在配合到合成树脂中时,在合成树脂组合物中优选为0.001~5质量%,更优选为0.05~3质量%。
作为上述受阻胺系光稳定剂,可列举出例如2,2,6,6-四甲基-4-哌啶基硬脂酸酯、1,2,2,6,6-五甲基-4-哌啶基硬脂酸酯、2,2,6,6-四甲基-4-哌啶基苯甲酸酯、双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(1,2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯、四(2,2,6,6-四甲基-4-哌啶基)-1,2,3,4-丁烷四羧酸酯、四(1,2,2,6,6-五甲基-4-哌啶基)-1,2,3,4-丁烷四羧酸酯、双(2,2,6,6-四甲基-4-哌啶基)/二(十三烷基)-1,2,3,4-丁烷四羧酸酯、双(1,2,2,6,6-五甲基-4-哌啶基)/二(十三烷基)-1,2,3,4-丁烷四羧酸酯、双(1,2,2,4,4-五甲基-4-哌啶基)-2-丁基-2-(3,5-二叔丁基-4-羟基苄基)丙二酸酯、1-(2-羟乙基)-2,2,6,6-四甲基-4-哌啶醇/琥珀酸二乙酯缩聚物、1,6-双(2,2,6,6-四甲基-4-哌啶基氨基)己烷/2,4-二氯-6-吗啉代-s-三嗪缩聚物、1,6-双(2,2,6,6-四甲基-4-哌啶基氨基)己烷/2,4-二氯-6-叔辛基氨基-s-三嗪缩聚物、1,5,8,12-四〔2,4-双(N-丁基-N-(2,2,6,6-四甲基-4-哌啶基)氨基)-s-三嗪-6-基〕-1,5,8,12-四氮杂十二烷、1,5,8,12-四〔2,4-双(N-丁基-N-(1,2,2,6,6-五甲基-4-哌啶基)氨基)-s-三嗪-6-基〕-1,5,8-12-四氮杂十二烷、1,6,11-三〔2,4-双(N-丁基-N-(2,2,6,6-四甲基-4-哌啶基)氨基)-s-三嗪-6-基〕氨基十一烷、1,6,11-三〔2,4-双(N-丁基-N-(1,2,2,6,6-五甲基-4-哌啶基)氨基)-s-三嗪-6-基〕氨基十一烷等受阻胺化合物。这些受阻胺系光稳定剂的使用量在配合到合成树脂中时,在合成树脂组合物中优选为0.001~5质量%,更优选为0.05~3质量%。
作为上述的抗老化剂,可列举出萘基胺系、二苯基胺系、对苯二胺系、喹啉系、氢醌衍生物、单酚系、硫代双酚系、受阻酚系、亚磷酸酯系等。这些抗老化剂的使用量在配合到合成树脂中时,在合成树脂组合物中优选为0.001~5质量%,更优选为0.05~3质量%。
在本发明的阻燃剂组合物中,在不损害本发明的效果的范围内,作为任意成分还可以配合增强材料。这些成分也可以在将本发明的阻燃剂组合物配合到合成树脂中时配合到合成树脂中。作为该增强材料,可以使用通常在合成树脂的增强中使用的纤维状、板状、粒状、粉末状的材料。具体而言,可列举出玻璃纤维、石棉纤维、碳纤维、石墨纤维、金属纤维、钛酸钾晶须、硼酸铝晶须、镁系晶须、硅系晶须、硅灰石、海泡石、石棉、矿渣纤维、硬硅钙石、硅磷灰石、石膏纤维、二氧化硅纤维、二氧化硅/氧化铝纤维、氧化锆纤维、氮化硼纤维、氮化硅纤维及硼纤维等无机纤维状增强材料、聚酯纤维、尼龙纤维、丙烯酸纤维、再生纤维素纤维、醋酸酯纤维、槿麻、苎麻、棉花、黄麻、麻、剑麻、亚麻、亚麻布、丝绸、马尼拉麻、甘蔗、木浆、纸屑、旧纸及羊毛等有机纤维状增强材料、玻璃薄片、非溶胀性云母、石墨、金属箔、陶瓷珠、粘土、云母、绢云母、沸石、膨润土、白云石、高岭土、微粉硅酸、长石粉、钛酸钾、二氧化硅微球、碳酸钙、碳酸镁、硫酸钡、氧化钙、氧化铝、氧化钛、硅酸铝、氧化硅、石膏、均密石英岩、片钠铝石及白土等板状或粒状的增强材料。这些增强材料也可以以乙烯/醋酸乙烯酯共聚物等热塑性树脂、或环氧树脂等热固化性树脂被覆或进行集束处理,也可以以氨基硅烷或环氧硅烷等偶联剂等进行处理。
在本发明的阻燃剂组合物中,在不损害本发明的效果的范围内,作为任意成分,还可以进一步配合晶核剂。作为该晶核剂,可以适当使用一般作为聚合物的晶核剂使用的晶核剂,本发明中,可以使用无机系晶核剂及有机系晶核剂中的任一种。这些成分也可以在将本发明的阻燃剂组合物配合到合成树脂中时配合到合成树脂中。
作为上述无机系晶核剂的具体例子,可列举出高岭石、合成云母、粘土、沸石、二氧化硅、石墨、炭黑、氧化镁、氧化钛、硫化钙、氮化硼、碳酸钙、硫酸钡、氧化铝、氧化钕及苯基膦酸盐等金属盐。为了提高在组合物中的分散性,这些无机系晶核剂也可以以有机物修饰。
作为上述有机系晶核剂的具体例子,可列举出苯甲酸钠、苯甲酸钾、苯甲酸锂、苯甲酸钙、苯甲酸镁、苯甲酸钡、对苯二甲酸锂、对苯二甲酸钠、对苯二甲酸钾、草酸钙、月桂酸钠、月桂酸钾、肉豆蔻酸钠、肉豆蔻酸钾、肉豆蔻酸钙、二十八烷酸钠、二十八烷酸钙、硬脂酸钠、硬脂酸钾、硬脂酸锂、硬脂酸钙、硬脂酸镁、硬脂酸钡、褐煤酸钠、褐煤酸钙、甲苯酸钠、水杨酸钠、水杨酸钾、水杨酸锌、二苯甲酸铝、二苯甲酸钾、二苯甲酸锂、β-萘二甲酸钠、环己烷羧酸钠等有机羧酸金属盐、对甲苯磺酸钠、间苯二甲酸磺酸钠等有机磺酸盐、硬脂酰胺、亚乙基双月桂酰胺、棕榈酰胺、羟基硬脂酰胺、芥酸酰胺、均苯三酸三(叔丁基酰胺)等羧酰胺、亚苄基山梨糖醇及其衍生物、2,2'-亚甲基双(4,6-二-叔丁基苯基)磷酸钠等磷化合物金属盐及2,2-甲基双(4,6-二-叔丁基苯基)钠等。
此外在本发明的阻燃性组合物中,在不损害本发明的效果的范围内,作为任意成分,还可以进一步配合丙烯酸系加工助剂。丙烯酸系加工助剂可以使用将(甲基)丙烯酸酯的一种聚合或将两种以上共聚而得到的物质。这些成分也可以在将本发明的阻燃剂组合物配合到合成树脂中时配合到合成树脂中。作为聚合或共聚的(甲基)丙烯酸酯的例子,可列举出丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸正丙酯、丙烯酸异丙酯、甲基丙烯酸正丙酯、甲基丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸异丁酯、甲基丙烯酸叔丁酯、丙烯酸正己酯、甲基丙烯酸正己酯、丙烯酸2-乙基己酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸十二烷基酯、甲基丙烯酸十三烷基酯等(甲基)丙烯酸酯等。此外,除了上述以外,还可列举出(甲基)丙烯酸、含有羟基的(甲基)丙烯酸酯。
在本发明的阻燃剂组合物中,在不损害本发明的效果的范围内,作为任意成分,还可以配合增塑剂。作为该增塑剂,可以适当使用一般作为聚合物的增塑剂使用的增塑剂,可列举出例如聚酯系增塑剂、甘油系增塑剂、多元羧酸酯系增塑剂、聚亚烷基二醇系增塑剂及环氧系增塑剂等。这些成分也可以在将本发明的阻燃剂组合物配合到合成树脂中时配合到合成树脂中。
作为上述聚酯系增塑剂的具体例子,可列举出由己二酸、癸二酸、对苯二甲酸、间苯二甲酸、萘二羧酸、二苯基二羧酸、松香等酸成分与丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇、乙二醇、二乙二醇等二醇成分构成的聚酯、或聚己内酯等由羟基羧酸构成的聚酯等。这些聚酯系增塑剂可以是以单官能羧酸或单官能醇将末端封端,此外也可以以环氧化合物等将末端封端。
作为上述甘油系增塑剂的具体例子,可列举出甘油单乙酰单月桂酸酯、甘油二乙酰单月桂酸酯、甘油单乙酰单硬脂酸酯、甘油二乙酰单油酸酯及甘油单乙酰单褐煤酸酯等。
作为上述多元羧酸酯系增塑剂的具体例子,可列举出邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、邻苯二甲酸二庚酯、邻苯二甲酸二苄酯、邻苯二甲酸丁基苄酯等邻苯二甲酸酯、偏苯三酸三丁酯、偏苯三酸三辛酯、偏苯三酸三己酯等偏苯三酸酯、己二酸二异癸酯、己二酸正辛基正癸酯、己二酸甲基二甘醇丁基二甘醇酯、己二酸苄基甲基二甘醇酯、己二酸苄基丁基二甘醇酯等己二酸酯、乙酰基柠檬酸三乙酯、乙酰基柠檬酸三丁酯等柠檬酸酯、壬二酸二-2-乙基己酯等壬二酸酯、癸二酸二丁酯及癸二酸二-2-乙基己酯等癸二酸酯等。
作为上述聚亚烷基二醇系增塑剂的具体例子,可列举出聚乙二醇、聚丙二醇、聚(环氧乙烷/环氧丙烷)嵌段和/或无规共聚物、聚四亚甲基二醇、双酚类的环氧乙烷加成聚合物、双酚类的环氧丙烷加成聚合物、双酚类的四氢呋喃加成聚合物等聚亚烷基二醇、或其末端环氧改性化合物、末端酯改性化合物及末端醚改性化合物等末端封端化合物等。
上述环氧系增塑剂一般是指由环氧硬脂酸烷基酯和大豆油构成的环氧三甘油酯等,但除此以外,还可以使用主要以双酚A和环氧氯丙烷作为原料那样的所谓的环氧树脂。
作为其他增塑剂的具体例子,可列举出新戊二醇二苯甲酸酯、二乙二醇二苯甲酸酯、三乙二醇二-2-乙基丁酸酯等脂肪族多元醇的苯甲酸酯、硬脂酰胺等脂肪酸酰胺、油酸丁酯等脂肪族羧酸酯、乙酰蓖麻油酸甲酯、乙酰蓖麻油酸丁酯等羟基酸酯、季戊四醇、各种山梨糖醇、聚丙烯酸酯及石蜡类等。
本发明中使用增塑剂的情况下,可以仅使用一种,也可以将两种以上并用。
此外,在本发明的阻燃剂组合物中,根据需要可以在不损害本发明的效果的范围内配合通常在合成树脂中使用的添加剂、例如交联剂、抗静电剂、金属皂、填充剂、防雾剂、防渗出剂、表面处理剂、荧光剂、防霉剂、杀菌剂、发泡剂、金属钝化剂、脱模剂、颜料、除丙烯酸系加工助剂以外的加工助剂等。这些成分也可以在将本发明的阻燃剂组合物配合到合成树脂中时配合到合成树脂中。
为了得到本发明的阻燃剂组合物,只要将必须成分的(A)~(C)成分、根据需要使用的(D)成分、进一步根据需要使用的其他任意成分混合即可,混合中可以使用各种混合机。也可以在混合时加热。若列举出可使用的混合机的例子,则可列举出转鼓混合机、亨舍尔混合机、螺条式搅拌机、V型混合机、W型混合机、高速混合机、诺塔混合机等。
本发明的阻燃剂组合物对合成树脂的阻燃化有效果,优选配合到合成树脂中制成阻燃性合成树脂组合物(以下,也称为本发明的阻燃性合成树脂组合物)使用。
作为通过本发明的阻燃剂组合物而阻燃化的合成树脂的具体例子,可列举出聚丙烯、高密度聚乙烯、低密度聚乙烯、直链低密度聚乙烯、交联聚乙烯、超高分子量聚乙烯、聚丁烯-1、聚-3-甲基戊烯等α-烯烃聚合物或乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸乙酯共聚物、乙烯-丙烯共聚物等聚烯烃及它们的共聚物、聚氯乙烯、聚偏氯乙烯、氯化聚乙烯、氯化聚丙烯、聚偏氟乙烯、氯化橡胶、氯乙烯-乙酸乙烯酯共聚物、氯乙烯-乙烯共聚物、氯乙烯-偏氯乙烯共聚物、氯乙烯-偏氯乙烯-乙酸乙烯酯三元共聚物、氯乙烯-丙烯酸酯共聚物、氯乙烯-马来酸酯共聚物、氯乙烯-环己基马来酰亚胺共聚物等含卤素树脂;石油树脂、香豆酮树脂、聚苯乙烯、聚乙酸乙烯酯、丙烯酸树脂、聚甲基丙烯酸甲酯、聚乙烯醇、聚乙烯醇缩甲醛、聚乙烯醇缩丁醛;聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚对苯二甲酸环己烷二亚甲酯等聚对苯二甲酸亚烷基二醇酯、聚萘二甲酸乙二醇酯、聚萘二甲酸丁二醇酯等聚萘二甲酸亚烷基二醇酯等芳香族聚酯及聚对苯二甲酸丁二醇酯等直链聚酯;聚羟基丁酸酯、聚己内酯、聚丁二酸丁二醇酯、聚丁二酸乙二醇酯、聚乳酸树脂、聚苹果酸、聚乙醇酸、聚二噁烷、聚(2-氧杂环丁酮)等分解性脂肪族聚酯;聚苯醚、聚己内酰胺及聚己二酰己二胺等聚酰胺、聚碳酸酯、支链聚碳酸酯、聚缩醛、聚苯硫醚、聚氨酯、纤维素系树脂等热塑性树脂及它们的共混物或者酚醛树脂、脲醛树脂、三聚氰胺树脂、环氧树脂、不饱和聚酯树脂等热固化性树脂、氟系树脂、硅酮树脂、硅橡胶、聚醚砜、聚砜、聚苯醚、聚醚酮、聚醚醚酮、液晶聚合物等。还可列举出异戊二烯橡胶、丁二烯橡胶、丙烯腈-丁二烯共聚橡胶、苯乙烯-丁二烯共聚橡胶、氟橡胶、硅橡胶等。
若进一步列举出阻燃化的合成树脂的具体例子,则可列举出烯烃系热塑性弹性体、苯乙烯系热塑性弹性体、聚酯系热塑性弹性体、腈系热塑性弹性体、尼龙系热塑性弹性体、氯乙烯系热塑性弹性体、聚酰胺系热塑性弹性体、聚氨酯系热塑性弹性体等。
这些合成树脂可以使用1种,也可以使用两种以上。此外合成树脂也可以被合金化。
本发明中使用的合成树脂不论分子量、聚合度、密度、软化点、在溶剂中的不溶成分的比例、立构规整性的程度、催化剂残渣的有无、作为原料的单体的种类或配合比率、聚合催化剂的种类(例如齐格勒催化剂、茂金属催化剂等)等如何,都可以使用。
这些合成树脂中,从能够赋予优异的阻燃性的方面出发,优选聚烯烃系树脂。
若列举出聚烯烃系树脂的例子,则可列举出例如聚乙烯、低密度聚乙烯、直链状低密度聚乙烯、高密度聚乙烯、聚丙烯、均聚丙烯、无规共聚物聚丙烯、嵌段共聚物聚丙烯、抗冲击共聚物聚丙烯、高抗冲击共聚物聚丙烯、等规聚丙烯、间规聚丙烯、半等规聚丙烯、马来酸酐改性聚丙烯、聚丁烯、环烯烃聚合物、立构嵌段聚丙烯、聚-3-甲基-1-丁烯、聚-3-甲基-1-戊烯、聚-4-甲基-1-戊烯等α-烯烃聚合物、乙烯/丙烯嵌段或无规共聚物、乙烯-甲基丙烯酸甲酯共聚物、乙烯-醋酸乙烯酯共聚物等α-烯烃共聚物等。
本发明的阻燃性合成树脂组合物中,包含(A)成分、(B)成分、(C)成分、并进一步包含(D)成分时,从阻燃性的方面出发,(D)成分的合计含量优选为10质量%以上且低于50质量%,更优选为15质量%以上且低于40质量%,进一步更优选为18质量%以上且低于30质量%,最优选为20质量%以上且低于25质量%。若低于10质量%,则有时无法发挥充分的阻燃性,若为50质量%以上,则有时损害树脂本来的物性。
本发明的阻燃性合成树脂组合物通过进行成形,可以得到阻燃性优异的成形品。成形方法没有特别限定,可列举出挤出加工、压延加工、注射成形、辊、压缩成形、吹塑成形等,可以制造树脂板、片材、膜、异形品等各种形状的成形品。
本发明的阻燃性合成树脂组合物可以用于电动汽车、机械、电气/电子设备、OA设备等的外壳(框架、框体、外壳、外包装)或部件、汽车内外装饰材料等中,被用于需要UL945VA的标准的用途中。
本发明的阻燃性合成树脂组合物及其成形体可以用于电气/电子/通信、农林水产、矿业、建设、食品、纤维、衣类、医疗、煤炭、石油、橡胶、皮革、汽车、精密设备、木材、建材、土木、家具、印刷、乐器等广泛的产业领域。更具体而言,可以用于打印机、电脑、文字处理机、键盘、PDA(小型信息终端机)、电话机、复印机、传真、ECR(电子式收银机)、计算器、电子笔记本、卡、架子、文具等办公用品、OA设备、洗衣机、冰箱、吸尘器、微波炉、照明器具、游戏机、电熨斗、被炉等家电设备、TV、VTR、摄像机、收录机、录音机、微型磁盘、CD播放器、扩音器、液晶显示器等AV设备、连接器、继电器、电容器、开关、印刷基板、线圈骨架、半导体密封材料、LED密封材料、电线、电缆、变压器、偏转轭、配电盘、钟表等电气/电子部件及通信设备、OA设备等的箱体(框架、框体、外壳、外包装)或部件、汽车内外装饰材料的用途。
进而,本发明的阻燃性合成树脂组合物及其成形体可以用于座位(填充物、内饰件等)、带、顶篷、活顶车顶篷、扶手、车门内饰、后杂物箱、地毯、垫子、遮阳板、轮毂装饰罩、垫子罩、安全气囊、绝缘材料、吊环、吊环带、电线被覆材料、电绝缘材料、涂料、涂布材料、外部装潢材料、地板材料、角壁、地毯、壁纸、壁装饰材料、外装饰材料、内装饰材料、屋顶材料、甲板材料、壁材、柱材、铺板、围墙的材料、骨架及造型、窗户及门的型材、木瓦、板壁、阳台、露台、防音板、绝热板、窗户材料等汽车、混合动力车、电动车、车辆、船舶、航空器、建筑物、住宅及建筑用材料、或土木材料、衣料、窗帘、床单、胶合板、合成纤维板、绒毯、玄关垫、片材、桶、软管、容器、眼镜、包、盒子、护目镜、滑雪板、球拍、帐篷、乐器等生活用品、体育用品等各种用途。
实施例
以下,通过实施例详细示出本发明。但是,本发明并不受以下的实施例的任何限制。另外,表1~4的配合全部为质量基准。
〔实施例1~6及比较例1~5〕
以表1记载的配方调制本发明的阻燃剂组合物。(C)成分的上述通式(1)所表示的二环磷酸酯化合物使用下述结构的化合物No.1。
化合物No.1
同样地以表2记载的配方调制阻燃剂组合物的比较例。比较例中还进行了使用聚磷酸铵来代替本发明的(B)成分的比较。
表1
*1:焦磷酸三聚氰胺的焦磷酸与三聚氰胺的比以摩尔比计为1:2。
*2:焦磷酸哌嗪的焦磷酸与哌嗪的比以摩尔比计为1:1。
表2
*1:焦磷酸三聚氰胺的焦磷酸与三聚氰胺的比以摩尔比计为1:2。
*2:焦磷酸哌嗪的焦磷酸与哌嗪的比以摩尔比计为1:1。
〔实施例7~15及比较例6~15〕
相对于在聚丙烯(熔体流动速率=8g/10min)60质量份中配合硬脂酸钙(润滑剂)0.1质量份、四[3-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯]甲烷(酚系抗氧化剂)0.1质量份、三(2,4-二叔丁基苯基)亚磷酸酯(磷系抗氧化剂)0.1质量份、甘油单硬脂酸酯(润滑剂)0.3质量份而得到的聚丙烯树脂组合物,以表3记载的配合比例(质量%)添加实施例1~6中得到的阻燃性组合物而得到实施例7~15的阻燃性合成树脂组合物。附带说一下,阻燃剂组合物是将实施例1中得到的阻燃剂组合物记为阻燃剂组合物-1,将实施例2中得到的阻燃剂组合物记为阻燃剂组合物-2,以下同样地使用直到实施例6中得到的阻燃剂组合物-6。
此外将比较例1中得到的阻燃剂组合物记为比较阻燃剂组合物-1,将比较例2中得到的阻燃性组合物记为比较阻燃剂组合物-2,以下同样地使用直到比较阻燃剂组合物-5,以表4记载的配合比例(质量%)添加而得到比较例6~15的比较阻燃性合成树脂组合物。
将所得到的阻燃性合成树脂组合物使用双螺杆挤出机(株式会社日本制钢所制TEX-28)以230℃、9kg/小时的条件挤出来制造粒料,使用其在200℃下进行注射成型,得到长度为127mm、宽度为12.7mm、厚度为1.6mm的试验片。使用该试验片进行阻燃性试验,以下述试验方法进行UL-94V试验。将结果示于表3及表4中。
此外,将上述阻燃性合成树脂组合物使用双螺杆挤出机(株式会社日本制钢所制TEX-28)以230℃、13kg/小时的条件挤出,制造加工性评价用的粒料。通过目视确认所得到的加工性评价用的粒料的表面状态,按照以下的评价基准确认发泡的有无,进行加工性的评价。将结果示于表3及表4中。
<阻燃性UL-94V试验方法>
将长度为127mm、宽度为12.7mm、厚度为1.6mm的试验片垂直地保持,对下端用燃烧器的火点10秒钟后,拿去火焰,测定试验片上点着的火熄灭的时间。接着,在火熄灭的同时进行第二次的点火10秒钟,与第一次同样地测定点着的火熄灭的时间。此外,同时还对试验片下面的棉条是否因为落下的火种而着火进行评价。
根据第一次和第二次的燃烧时间、棉条有无着火等,按照UL-94V标准来确定燃烧等级。燃烧等级中,V-0为最高,按照V-1、V-2的顺序阻燃性依次下降。但是,将与V-0~V-2的等级均不相符的记为NR。
<加工性评价>
〇:在粒料的表面几乎没有发泡的痕迹,加工性良好。
△:在粒料的表面见到少数的发泡的痕迹。
×:在粒料的表面有许多发泡的痕迹,加工性差。
表3
表4
Claims (5)
1.一种阻燃剂组合物,其含有20~50质量份的下述(A)成分、50~80质量份的下述(B)成分、0.01~20.0质量份的下述(C)成分,其中,(A)成分和(B)成分的合计为100质量份,
(A)成分:选自正磷酸三聚氰胺、焦磷酸三聚氰胺、多磷酸三聚氰胺的组中的一种以上的三聚氰胺盐,
(B)成分:选自正磷酸哌嗪、焦磷酸哌嗪、多磷酸哌嗪的组中的一种以上的哌嗪盐,
(C)成分:下述通式(1)所表示的二环磷酸酯化合物,
式(1)中,R表示碳原子数为1~4的烷基、或碳原子数为1~4的羟基烷基,
所述通式(1)所表示的二环磷酸酯化合物为下述的化合物No.1~No.6,
化合物No.1
化合物No.2
化合物No.3
化合物No.4
化合物No.5
化合物No.6
2.根据权利要求1所述的阻燃剂组合物,其中,进一步含有0.01~10质量份的氧化锌作为(D)成分。
3.一种阻燃性合成树脂组合物,其在合成树脂中配合了权利要求1或2所述的阻燃剂组合物。
4.根据权利要求3所述的阻燃性合成树脂组合物,其中,合成树脂为聚烯烃系树脂。
5.一种成形体,其是由权利要求3或4所述的阻燃性合成树脂组合物得到的。
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CN (1) | CN107075378B (zh) |
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CN107207806B (zh) * | 2015-02-06 | 2020-07-28 | 株式会社艾迪科 | 阻燃性聚丙烯组合物 |
US20190256780A1 (en) * | 2016-07-29 | 2019-08-22 | Adeka Corporation | Flame-retardant composition and flame-retardant synthetic-resin composition |
CN109563410B (zh) * | 2016-08-29 | 2020-12-22 | 株式会社艾迪科 | 阻燃剂组合物及阻燃性合成树脂组合物 |
CN109844014B (zh) * | 2016-09-28 | 2022-04-01 | 日本瑞翁株式会社 | 氯乙烯树脂组合物、氯乙烯树脂成型体及层叠体 |
US11292892B2 (en) | 2017-05-25 | 2022-04-05 | Adeka Corporation | Flame retardant composition and flame retardant resin composition containing same |
WO2019021671A1 (ja) * | 2017-07-24 | 2019-01-31 | 株式会社Adeka | 組成物及び難燃性樹脂組成物 |
EP3683288B1 (en) * | 2017-09-12 | 2023-06-07 | Adeka Corporation | Composition and flame retardant resin composition |
KR20190032153A (ko) | 2017-09-18 | 2019-03-27 | 김성우 | 상수도용 저수조의 물순환 장치 |
CN111094515B (zh) * | 2017-09-28 | 2022-03-11 | 株式会社艾迪科 | 阻燃剂组合物、包含该阻燃剂组合物的阻燃性树脂组合物及该阻燃性树脂组合物的成形体 |
KR20200096912A (ko) * | 2017-12-14 | 2020-08-14 | 가부시키가이샤 아데카 | 조성물 및 난연성 수지 조성물 |
CN110157169A (zh) * | 2018-03-19 | 2019-08-23 | 李顺河 | 一种环保的阻燃可降解塑料 |
CN108440943A (zh) * | 2018-03-29 | 2018-08-24 | 苏州博莱特新材料有限公司 | 一种阻燃型水性聚氨酯树脂的制备方法 |
CN108440887A (zh) * | 2018-03-29 | 2018-08-24 | 苏州博莱特新材料有限公司 | 一种阻燃型水性丙烯酸树脂 |
CN108530576A (zh) * | 2018-03-29 | 2018-09-14 | 苏州博莱特新材料有限公司 | 一种阻燃型水性丙烯酸树脂的制备方法 |
KR102228985B1 (ko) * | 2019-03-27 | 2021-03-17 | 광성기업 주식회사 | 무스킨 선바이저 |
CN110423443B (zh) * | 2019-08-20 | 2021-06-29 | 湖南工业大学 | 一种生物质基高强韧阻燃板材 |
EP4158671A2 (en) * | 2020-05-27 | 2023-04-05 | Nohms Technologies, Inc. | Modified ionic liquids containing bicyclophosphate moiety |
CN112876739B (zh) * | 2021-01-22 | 2022-11-04 | 深圳市锦昊辉实业发展有限公司 | 一种无卤阻燃剂的制备方法及无卤阻燃剂、密封胶 |
CN113845725B (zh) * | 2021-10-19 | 2023-03-21 | 青岛塑科高分子科技有限公司 | 一种具有良好耐水性的阻燃聚丙烯材料及其制备方法 |
WO2023163710A1 (en) * | 2022-02-25 | 2023-08-31 | Hewlett-Packard Development Company, L.P. | Flame-resistant three-dimensional printed articles |
KR102509716B1 (ko) * | 2022-10-13 | 2023-03-14 | 주식회사 퍼시픽인터켐코포레이션 | 다기능성 가공 첨가제 |
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- 2015-10-27 CN CN201580062883.1A patent/CN107075378B/zh not_active Expired - Fee Related
- 2015-10-27 US US15/531,566 patent/US10513598B2/en not_active Expired - Fee Related
- 2015-10-27 WO PCT/JP2015/080259 patent/WO2016111074A1/ja active Application Filing
- 2015-10-27 KR KR1020177014270A patent/KR102456220B1/ko active IP Right Grant
- 2015-10-27 EP EP15876947.1A patent/EP3243890B1/en not_active Not-in-force
- 2015-11-06 TW TW104136726A patent/TWI680136B/zh active
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EP1120441B1 (en) * | 2000-01-26 | 2004-06-23 | Idemitsu Petrochemical Co., Ltd. | Flame-retardant and flame-retarding resin composition |
CN103298884A (zh) * | 2010-11-16 | 2013-09-11 | 路博润高级材料公司 | 非卤素阻燃热塑性聚氨酯 |
Also Published As
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TWI680136B (zh) | 2019-12-21 |
TW201625651A (zh) | 2016-07-16 |
KR102456220B1 (ko) | 2022-10-19 |
JP6448370B2 (ja) | 2019-01-09 |
EP3243890B1 (en) | 2019-01-09 |
WO2016111074A1 (ja) | 2016-07-14 |
US10513598B2 (en) | 2019-12-24 |
KR20170103754A (ko) | 2017-09-13 |
CN107075378A (zh) | 2017-08-18 |
JP2016125035A (ja) | 2016-07-11 |
EP3243890A1 (en) | 2017-11-15 |
EP3243890A4 (en) | 2018-08-15 |
US20170342239A1 (en) | 2017-11-30 |
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