CN114929801A - 阻燃剂组合物、阻燃性树脂组合物和成型体 - Google Patents
阻燃剂组合物、阻燃性树脂组合物和成型体 Download PDFInfo
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- CN114929801A CN114929801A CN202180008610.4A CN202180008610A CN114929801A CN 114929801 A CN114929801 A CN 114929801A CN 202180008610 A CN202180008610 A CN 202180008610A CN 114929801 A CN114929801 A CN 114929801A
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- flame retardant
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Abstract
提供:能对合成树脂赋予优异的阻燃性的阻燃剂组合物、具有优异的阻燃性、且耐水性和耐冲击性也优异的阻燃性树脂组合物;以及,其成型体。一种阻燃剂组合物,其含有下述(A)成分和下述(B)成分。(A)成分:含有下述(A‑1)~(A‑3)成分中的至少任一者的磷酸盐系阻燃剂,(A‑1)成分:选自由正磷酸三聚氰胺、焦磷酸三聚氰胺和多磷酸三聚氰胺组成的组中的1种以上的三聚氰胺盐,(A‑2)成分:选自由正磷酸哌嗪、焦磷酸哌嗪和多磷酸哌嗪组成的组中的1种以上的哌嗪盐,(A‑3)成分:选自由正磷酸铵、焦磷酸铵和多磷酸铵组成的组中的1种以上的铵盐,(B)成分:酸改性聚烯烃中的1种以上。
Description
技术领域
本发明涉及阻燃剂组合物、阻燃性树脂组合物(以下,也简称为“树脂组合物”)和成型体,详细而言,涉及对合成树脂赋予优异的阻燃性的阻燃剂组合物、具有优异的阻燃性、且耐水性和耐冲击性也优异的阻燃性树脂组合物、以及其成型体。
背景技术
合成树脂由于优异的化学特性和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、家电制品的壳体材料、玩具等。然而,大多合成树脂为可燃性,根据用途需要用于降低火灾的危险性的阻燃化。特别是,以聚烯烃树脂为代表的具有高可燃性的合成树脂在广泛的领域被大量使用,因此,在这些树脂中不可避免地配混用于赋予阻燃性的阻燃剂。
作为一直以来使用的合成树脂用的阻燃剂,有:卤素系阻燃剂、金属氢氧化物、磷系阻燃剂、作为阻燃助剂的氧化锑、三聚氰胺化合物等,广泛已知将它们单独使用或组合而使用。
然而,卤素系阻燃剂具有燃烧时产生的卤化氢气体、产烟量多之类的问题,金属氢氧化物需要大量的添加,因此,存在所配混的树脂的比重增加、机械特性降低之类的问题。因此,尝试了使用不产生这些问题的磷系阻燃剂。特别是,多磷酸铵、多磷酸与胺的盐所构成的磷酸盐系阻燃剂由于其优异的阻燃性能、低产烟性、低毒性之类的很多优点而被广泛使用。
另一方面,由于这些磷酸盐系阻燃剂具有水溶性,因此,在配混有该阻燃剂的树脂组合物被暴露于水中时,阻燃剂成分溶出,存在引起阻燃性降低、外观不良等耐水性降低的问题。
作为解决耐水性的问题的方法,专利文献1中公开了一种阻燃性树脂组合物,其配混有磷酸盐系阻燃剂与聚碳二亚胺。
现有技术文献
专利文献
专利文献1:日本专利第5424444号公报
发明内容
发明要解决的问题
上述专利文献1中记载的发明具有抑制将试验片浸渍于热水时的成分溶出量的效果,但近年来,期望实现能发挥进一步优异的耐水性能的技术。
因此,本发明的目的在于,提供:能对合成树脂赋予优异的阻燃性的阻燃剂组合物、通过含有该阻燃剂组合物而具有优异的阻燃性、且耐水性和耐冲击性也优异的阻燃性树脂组合物、以及其成型体。
用于解决问题的方案
本发明人等进行了深入研究,结果发现:通过形成下述构成,从而可以解决上述课题,至此完成了本发明。
即,本发明提供一种阻燃剂组合物,其特征在于,含有下述(A)成分和下述(B)成分。
(A)成分:含有下述(A-1)~(A-3)成分中的至少任一者的磷酸盐系阻燃剂
(A-1)成分:选自由正磷酸三聚氰胺、焦磷酸三聚氰胺和多磷酸三聚氰胺组成的组中的1种以上的三聚氰胺盐
(A-2)成分:选自由正磷酸哌嗪、焦磷酸哌嗪和多磷酸哌嗪组成的组中的1种以上的哌嗪盐
(A-3)成分:选自由正磷酸铵、焦磷酸铵和多磷酸铵组成的组中的1种以上的铵盐
(B)成分:酸改性聚烯烃中的1种以上
本发明的阻燃剂组合物优选相对于前述(A)成分100质量份,含有前述(B)成分0.5~75质量份。另外,本发明的阻燃剂组合物中,前述(B)成分优选为选自马来酸改性聚烯烃和马来酸酐改性聚烯烃中的1种以上。
进一步,本发明的阻燃剂组合物中,优选前述(B)成分的酸改性聚烯烃的酸值为1~100mgKOH/g。进一步另外,本发明的阻燃剂组合物中,还优选前述(B)成分的酸改性聚烯烃的质均分子量以聚苯乙烯换算计为1000~500000。
进一步另外,本发明的阻燃剂组合物优选还含有选自由硅油、环氧系偶联剂和润滑剂组成的组中的至少1种作为(C)成分,还优选还含有氧化锌作为(D)成分。
本发明的阻燃性树脂组合物的特征在于,在合成树脂中含有上述本发明的阻燃剂组合物。本发明的阻燃性树脂组合物中,优选相对于前述合成树脂100质量份,含有前述阻燃剂组合物10~400质量份。
本发明的阻燃性树脂组合物中,前述合成树脂优选为选自由烯烃系树脂、苯乙烯系树脂、乙酸乙烯酯系树脂和它们的共聚物组成的组中的1种以上。
本发明的成型体的特征在于,其是由上述本发明的阻燃性树脂组合物得到的。
发明的效果
根据本发明,可以提供对合成树脂赋予优异的阻燃性的阻燃剂组合物。另外,根据本发明,可以提供具有优异的阻燃性、且耐水性、耐冲击性也优异的阻燃性树脂组合物和其成型体。
具体实施方式
本发明涉及阻燃剂组合物、阻燃性树脂组合物和成型体。以下,基于其优选的实施方式对本发明进行说明。
<阻燃剂组合物>
本发明的阻燃剂组合物含有下述(A)成分和下述(B)成分。
(A)成分:磷酸盐系阻燃剂
(B)成分:酸改性聚烯烃中的1种以上
((A)成分)
本发明的作为(A)成分的磷酸盐系阻燃剂含有下述(A-1)~(A-3)成分中的至少任一者。
(A-1)成分:选自由正磷酸三聚氰胺、焦磷酸三聚氰胺和多磷酸三聚氰胺组成的组中的1种以上的三聚氰胺盐
(A-2)成分:选自由正磷酸哌嗪、焦磷酸哌嗪和多磷酸哌嗪组成的组中的1种以上的哌嗪盐
(A-3)成分:选自由正磷酸铵、焦磷酸铵和多磷酸铵组成的组中的1种以上的铵盐
本发明的(A)成分中,作为(A-1)成分使用的三聚氰胺盐选自由正磷酸三聚氰胺、焦磷酸三聚氰胺和多磷酸三聚氰胺组成的组,它们可以单独使用也可以以混合物的形式使用。这些之中,从阻燃性、操作性和保存稳定性的方面出发,优选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。以混合物的形式使用它们的情况下,焦磷酸三聚氰胺的含有比例越高越优选。另外,焦磷酸三聚氰胺中的、焦磷酸与三聚氰胺的比以摩尔比计优选1:2。
这些磷酸类与三聚氰胺的盐也可以分别通过使对应的磷酸类或磷酸类的盐与三聚氰胺进行反应而得到,作为本发明的(A-1)成分中使用的三聚氰胺盐,优选使正磷酸三聚氰胺进行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(A)成分中,作为(A-2)成分使用的哌嗪盐选自由正磷酸哌嗪、焦磷酸哌嗪和多磷酸哌嗪组成的组,它们可以单独使用也可以以混合物的形式使用。这些之中,从阻燃性、操作性和保存稳定性的方面出发,优选焦磷酸哌嗪,以混合物的形式使用的情况下,焦磷酸哌嗪的含有比例越高越优选。另外,焦磷酸哌嗪中的、焦磷酸与哌嗪的比以摩尔比计优选1:1。
这些磷酸类与哌嗪的盐也可以通过分别使对应的磷酸类或磷酸类的盐与哌嗪进行反应而得到,作为本发明的(A-2)成分中使用的哌嗪盐,优选使二磷酸哌嗪进行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。
本发明的(A)成分中,作为(A-3)成分使用的铵盐选自由正磷酸铵、焦磷酸铵和多磷酸铵组成的组,它们可以单独使用也可以以混合物的形式使用。这些之中,从阻燃性的方面出发,优选多磷酸铵。
另外,上述铵盐单体容易受到水解,因此,也可以适合使用:将上述铵盐用热固化性树脂覆盖或微囊化而成者、用三聚氰胺单体、其他含氮有机化合物等覆盖上述铵盐颗粒而成者,此外,也可以使用:用表面活性剂、或硅烷偶联剂、硅油等有机硅化合物进行了处理而成者、制造上述铵盐的过程中添加三聚氰胺等并难溶化而成者等。
从阻燃性的方面出发,本发明的(A)成分特别优选含有(A-1)成分和(A-2)成分。该情况下,对于(A-1)成分与(A-2)成分的含有比例,从阻燃性的方面出发,以(A-1)成分与(A-2)成分的质量比计、优选20:80~50:50、更优选30:70~45:55。
((B)成分)
本发明的(B)成分为酸改性聚烯烃中的1种以上。
酸改性聚烯烃是在聚烯烃中导入马来酸酐等酸性基团而得到的聚合物。
酸改性聚烯烃可以通过使具有酸性基团的单体与聚烯烃进行接枝化反应的方法、使具有酸性基团的单体与烯烃单体进行共聚的方法等以往公知的方法而得到,也可以使用各种市售品。
上述聚烯烃是1种以上的烯烃单体经聚合或共聚而得到的。作为烯烃单体,例如可以举出乙烯、丙烯、α-烯烃或二烯,作为α-烯烃,例如可以举出1-丁烯、4-甲基-1-戊烯、1-戊烯、1-辛烯、1-癸烯、1-十二碳烯等,作为二烯,例如可以举出丁二烯、异戊二烯、环戊二烯、1,11-十二碳二烯等。另外,除这些以外也可以包含其他共聚成分。作为由这些构成的聚烯烃,具体而言,可以举出聚乙烯、聚丙烯、乙烯-丙烯共聚物、乙烯-丙烯-二烯三元共聚物、乙烯-1-丁烯共聚物、乙烯-乙酸乙烯酯共聚物、和它们的混合物等。上述中,从树脂组合物的耐水性和力学特性的方面出发,优选乙烯、丙烯、碳原子数4~12的α-烯烃、丁二烯、异戊二烯经聚合或共聚而成者,更优选乙烯、丙烯、碳原子数4~8的α-烯烃、丁二烯经聚合或共聚而成者,进一步更优选乙烯、丙烯、丁二烯经聚合或共聚而成者。
作为导入至酸改性聚烯烃的上述酸性基团,可以举出羧酸基、羧酸酐基、磺酸基、磷酸基等,从抑制树脂组合物的劣化的方面出发,优选羧酸基、羧酸酐基。
作为具有上述酸性基团的单体,可以举出羧酸化合物、羧酸酐化合物、磺酸化合物、磷酸化合物等,从抑制树脂组合物的劣化的方面出发,优选羧酸化合物、羧酸酐化合物,更优选马来酸、马来酸酐、丙烯酸、甲基丙烯酸,特别优选马来酸、马来酸酐。
作为属于本发明的(B)成分的酸改性聚烯烃,从树脂组合物中的耐水性、力学特性和抑制劣化的方面出发,优选为选自羧酸改性聚烯烃和羧酸酐改性聚烯烃中的1种以上,更优选为选自马来酸改性聚烯烃和马来酸酐改性聚烯烃中的1种以上,进一步更优选为选自马来酸改性聚乙烯、马来酸酐改性聚乙烯、马来酸改性聚丙烯和马来酸酐改性聚丙烯中的1种以上,特别优选为选自马来酸改性聚乙烯和马来酸酐改性聚乙烯中的1种以上。
从树脂组合物中的耐水性、力学特性和抑制劣化的方面出发,酸改性聚烯烃的酸值优选1~100mgKOH/g、更优选2~80mgKOH/g、最优选5~70mgKOH/g的范围。该酸值是依据JIS K 0070、按照以下的(i)~(iii)的步骤测定而得到的值。
[酸改性聚烯烃的酸值测定方法]
(i)使酸改性聚烯烃1g溶解于加热至140℃的二甲苯70ml。
(ii)在同一温度下,将酚酞作为指示剂,用0.1mol/L氢氧化钾乙醇溶液(商品名“0.1mol/L乙醇性氢氧化钾溶液”、和光纯药株式会社制)进行滴定。
(iii)将滴定所需的氢氧化钾量换算为mg,算出酸值(单位:mgKOH/g)。
另外,从含有本发明的阻燃剂组合物的树脂组合物中的力学特性的方面出发,酸改性聚烯烃的质均分子量(Mw)以聚苯乙烯换算计优选为1000~500000、更优选5000~300000、进一步更优选20000~210000。该质均分子量是依据JIS K 7252-1、通过尺寸排阻色谱法而测定的、以聚苯乙烯换算计所示的值。
本发明的阻燃剂组合物中,(B)成分相对于(A)成分100质量份的含有比例优选0.5~75质量份、更优选1~65质量份、进一步更优选3~55质量份。通过使(B)成分相对于(A)成分100质量份的含有比例为上述范围,从而可以充分得到本发明的效果,不会对含有本发明的阻燃剂组合物的树脂组合物的力学特性、劣化抑制造成不良影响,因而优选。
((C)成分)
本发明的阻燃剂组合物中,优选还含有选自由硅油、环氧系偶联剂和润滑剂组成的组中的至少1种作为(C)成分。
本发明的阻燃剂组合物中含有上述(C)成分,从而可以抑制阻燃剂粉末聚集的情况,可以期待保存稳定性的改善、和对合成树脂的分散性改善、阻燃性改善。
作为上述硅油的例子,可以举出聚硅氧烷的侧链和末端全部为甲基的二甲基硅油、聚硅氧烷的侧链和末端为甲基、其侧链的一部分为苯基的甲基苯基硅油、聚硅氧烷的侧链和末端为甲基、其侧链的一部分为氢的甲基氢硅油等、它们的共聚物,另外,可以使用在这些侧链和/或末端的一部分中导入有机基团,进行了胺改性、环氧改性、脂环式环氧改性、羧基改性、甲醇改性、巯基改性、聚醚改性、长链烷基改性、氟烷基改性、高级脂肪酸酯改性、高级脂肪酸酰胺改性、硅烷醇基改性、二醇改性、苯酚改性和/或芳烷基改性而得到的改性硅油。
如果列举上述硅油的具体例,则作为二甲基硅油,可以举出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,可以举出KF-99(信越化学株式会社制)、KF-9901(信越化学株式会社制)、HMS-151(Gelest公司制)、HMS-071(Gelest公司制)、HMS-301(Gelest公司制)、DMS-H21(Gelest公司制)等,作为甲基苯基硅油的例子,可以举出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,作为环氧改性品,例如可以举出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,例如可以举出X-22-3701E(信越化学株式会社制),作为甲醇改性品,例如可以举出X-22-4039(信越化学株式会社制)、X-22-4015(信越化学株式会社制),作为胺改性品,例如可以举出KF-393(信越化学株式会社制)等。
本发明的阻燃剂组合物的上述硅油中,从防止阻燃剂粉末聚集的情况、实现保存稳定性的改善和对合成树脂的分散性改善的方面出发,优选甲基氢硅油。
上述环氧系偶联剂具有抑制阻燃剂粉末的聚集、改善保存稳定性且赋予耐水性和耐热性的功能。作为上述环氧系偶联剂,例如可以举出通式A-(CH2)k-Si(OR)3所示的化合物、且具有环氧基的化合物。上述式中,A表示具有环氧基的基团,k表示1~3的整数,R表示甲基或乙基。作为此处所谓具有环氧基的基团,可以举出环氧丙氧基、3,4-环氧环己基。
作为上述环氧系偶联剂的具体例,例如作为具有环氧基的硅烷偶联剂,可以举出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。
作为上述润滑剂,可以举出液体石蜡、天然石蜡、微晶蜡、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、氧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、脂肪酸与多元醇的偏酯、脂肪酸与聚二醇、聚甘油的偏酯系的润滑剂、硅油、矿物油等。润滑剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中含有上述(C)成分的情况下,从有效地发挥含有上述(C)成分的效果的观点出发,本发明的阻燃剂组合物中的(C)成分的含量相对于上述(A)成分100质量份,优选0.01~5质量份、更优选0.01~3质量份。
特别是,从提高含有硅油所产生的上述效果的方面出发,本发明的阻燃剂组合物中含有硅油时的硅油的含量相对于上述(A)成分100质量份,优选0.01~3质量份、更优选0.1~1质量份。
特别是,从提高含有环氧系偶联剂所产生的上述效果的方面出发,本发明的阻燃剂组合物中含有环氧系偶联剂时的环氧系偶联剂的含量相对于上述(A)成分100质量份,优选0.01~3质量份、更优选0.1~1质量份。
特别是,从提高含有润滑剂所产生的上述效果的方面出发,本发明的阻燃剂组合物中含有润滑剂时的润滑剂的含量相对于上述(A)成分100质量份,优选0.01~3质量份、更优选0.1~0.5质量份。
((D)成分)
本发明的阻燃剂组合物中,优选还含有氧化锌作为(D)成分。
上述氧化锌作为阻燃助剂发挥功能。氧化锌有时进行表面处理。氧化锌可以使用市售品,例如可以举出氧化锌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0.02μm的超细粒氧化锌:堺化学工业株式会社制)、NANOFINE K(用平均粒径0.02μm的硅酸锌覆膜而得到的超细粒氧化锌:堺化学工业株式会社制)等。
本发明的阻燃剂组合物中,从改善阻燃性的方面出发,作为上述(D)成分的氧化锌的含量相对于上述(A)成分100质量份,优选0.01~20质量份、更优选0.5~10质量份、进一步优选1~5质量份。通过将氧化锌的含量设定为0.01质量份以上,从而阻燃性变得更良好。另一方面,通过将氧化锌的含量设定为20质量份以下,从而不易对加工性产生不良影响。
(其他成分)
本发明的阻燃剂组合物中,在不显著有损本发明的效果的范围内,可以任意含有公知的树脂添加剂。作为这种树脂添加剂,例如可以使用选自酚系抗氧化剂、磷系抗氧化剂、硫醚系抗氧化剂、其他抗氧化剂、受阻胺系光稳定剂、紫外线吸收剂、增塑剂、结晶成核剂、本发明的磷酸盐系阻燃剂以外的阻燃剂、阻燃助剂、防滴落剂、丙烯酸类加工助剂、填充剂、水滑石类、金属皂、抗静电剂、颜料和染料中的1种以上。这些树脂添加剂可以预先配混在本发明的阻燃剂组合物中,也可以在制备后述的阻燃性树脂组合物时配混。
作为上述酚系抗氧化剂,例如可以举出:2,6-二叔丁基-对甲酚、2,6-二苯基-4-十八烷氧基苯酚、硬脂基(3,5-二叔丁基-4-羟基苯基)丙酸酯、二硬脂基(3,5-二叔丁基-4-羟基苄基)膦酸酯、十三烷基·3,5-二叔丁基-4-羟基苄基硫代乙酸酯、硫代二乙烯双[(3,5-二叔丁基-4-羟基苯基)丙酸酯]、4,4’-硫代双(6-叔丁基-间甲酚)、2-辛基硫代-4,6-双(3,5-二叔丁基-4-羟基苯氧基)-均三嗪、2,2’-亚甲基双(4-甲基-6-叔丁基苯酚)、乙烯双[3,3-双(4-羟基-3-叔丁基苯基)丁酸酯]、4,4’-丁叉基双(2-叔丁基-5-甲基苯酚)、2,2’-乙叉基双(4,6-二叔丁基苯酚)、1,1,3-三(2-甲基-4-羟基-5-叔丁基苯基)丁烷、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(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、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、四[亚甲基-3-(3,5-二叔丁基-4-羟基苯基)丙酸酯]甲烷、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、3,9-双[2-{3-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基}-1,1-二甲基乙基]-2,4,8,10-四氧杂螺[5.5]十一烷、三乙二醇双[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯]等。这些酚系抗氧化剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的酚系抗氧化剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.01~1质量份的量,更优选成为0.03~0.8质量份的量。
作为上述磷系抗氧化剂,例如可以举出:亚磷酸三苯酯、亚磷酸二异辛酯、七(二丙二醇)三亚磷酸酯、亚磷酸三异癸酯、亚磷酸二苯基异辛酯、亚磷酸二异辛基苯酯、亚磷酸二苯基十三烷酯、亚磷酸三异辛酯、亚磷酸三月桂酯、亚磷酸二苯酯、三(二丙二醇)亚磷酸酯、二异癸基季戊四醇二亚磷酸酯、二油烯基氢亚磷酸酯、三月桂基三硫代亚磷酸酯、双(十三烷基)亚磷酸酯、三(十三烷基)亚磷酸酯、亚磷酸二苯基癸酯、二壬基苯基双(壬基苯基)亚磷酸酯、聚(二丙二醇)苯基亚磷酸酯、四苯基二丙二醇二亚磷酸酯、三(壬基苯基)亚磷酸酯、三(2,4-二叔丁基苯基)亚磷酸酯、三(2,4-二叔丁基-5-甲基苯基)亚磷酸酯、三〔2-叔丁基-4-(3-叔丁基-4-羟基-5-甲基苯基硫代)-5-甲基苯基〕亚磷酸酯、三癸基亚磷酸酯、辛基二苯基亚磷酸酯、二癸基单苯基亚磷酸酯、二硬脂基季戊四醇二亚磷酸酯、二硬脂基季戊四醇二亚磷酸酯与硬脂酸钙盐的混合物、双(十三烷基)季戊四醇二亚磷酸酯、双(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、四苯基四(十三烷基)季戊四醇四亚磷酸酯、双(2,4-二叔丁基-6-甲基苯基)乙基亚磷酸酯、四(十三烷基)异丙叉基二苯酚二亚磷酸酯、四(十三烷基)-4,4’-正丁叉基双(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-5-叔丁基苯基)丁烷三亚磷酸酯、四(2,4-二叔丁基苯基)亚联苯基二亚膦酸酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、(1-甲基-1-丙烯基-3-叉基)三(1,1-二甲基乙基)-5-甲基-4,1-亚苯基)六(十三烷基)亚磷酸酯、2,2’-亚甲基双(4,6-二叔丁基苯基)-2-乙基己基亚磷酸酯、2,2’-亚甲基双(4,6-二叔丁基苯基)十八烷基亚磷酸酯、2,2’-乙叉基双(4,6-二叔丁基苯基)氟亚磷酸酯、4,4’-丁叉基双(2-叔丁基-5-甲基苯基)四(十三烷基)双亚磷酸酯、三(2-〔(2,4,8,10-四-叔丁基二苯并[d,f][1,3,2]二氧杂膦杂-6-基)氧基〕乙基)胺、3,9-双(4-壬基苯氧基)-2,4,8,10-四氧杂-3,9-二磷杂螺[5,5]十一烷、2,4,6-三叔丁基苯基-2-丁基-2-乙基-1,3-丙二醇亚磷酸酯、4,4’-异丙叉基二苯酚C10醇亚磷酸酯、4,4’-异丙叉基二苯酚C12-15醇亚磷酸酯等。这些磷系抗氧化剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的磷系抗氧化剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.01~1质量份的量,更优选成为0.03~0.8质量份的量。
作为上述硫代醚系抗氧化剂,例如可以举出四[亚甲基-3-(月桂基硫代)丙酸酯]甲烷、双(甲基-4-[3-正烷基(C12/C14)硫代丙酰氧基]5-叔丁基苯基)硫醚、双(十三烷基)-3,3’-硫代二丙酸酯、二月桂基-3,3’-硫代二丙酸酯、二肉豆蔻基-3,3’-硫代二丙酸酯、二硬脂基-3,3’-硫代二丙酸酯、月桂基/硬脂基硫代二丙酸酯、4,4’-硫代双(6-叔丁基-间甲酚)、2,2’-硫代双(6-叔丁基-对甲酚)、二硬脂基-二硫醚。这些硫代醚系抗氧化剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的硫代醚系抗氧化剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.001~10质量份的量,更优选成为0.005~5质量份的量。
作为上述受阻胺系光稳定剂,例如可以举出: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、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)·双(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-羟基乙基)-2,2,6,6-四甲基-4-羟基哌啶/琥珀酸二乙基缩聚物、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-均三嗪缩聚物、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-均三嗪缩聚物、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)-均三嗪-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)-均三嗪-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)-均三嗪-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)-均三嗪-6-基〕氨基十一烷、双(2,2,6,6-四甲基-1-辛氧基-4-哌啶基)癸二酸酯、双(2,2,6,6-四甲基-1-十一烷氧基哌啶-4-基)碳酸酯、CibaSpecialty Chemicals公司制TINUVIN NOR371等。这些受阻胺系光稳定剂可以单独使用1种,也可以并用2种以上而使用。
这些受阻胺系光稳定剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.001~10质量份的量,更优选成为0.005~1质量份的量。
作为上述紫外线吸收剂,例如可以举出:2,4-二羟基二苯甲酮、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-5-叔辛基苯基)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-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)苯并三唑的聚乙二醇酯、2-〔2-羟基-3-(2-丙烯酰氧基乙基)-5-甲基苯基〕苯并三唑、2-〔2-羟基-3-(2-甲基丙烯酰氧基乙基)-5-叔丁基苯基〕苯并三唑、2-〔2-羟基-3-(2-甲基丙烯酰氧基乙基)-5-叔辛基苯基〕苯并三唑、2-〔2-羟基-3-(2-甲基丙烯酰氧基乙基)-5-叔丁基苯基〕-5-氯苯并三唑、2-〔2-羟基-5-(2-甲基丙烯酰氧基乙基)苯基〕苯并三唑、2-〔2-羟基-3-叔丁基-5-(2-甲基丙烯酰氧基乙基)苯基〕苯并三唑、2-〔2-羟基-3-叔戊基-5-(2-甲基丙烯酰氧基乙基)苯基〕苯并三唑、2-〔2-羟基-3-叔丁基-5-(3-甲基丙烯酰氧基丙基)苯基〕-5-氯苯并三唑、2-〔2-羟基-4-(2-甲基丙烯酰氧基甲基)苯基〕苯并三唑、2-〔2-羟基-4-(3-甲基丙烯酰氧基-2-羟基丙基)苯基〕苯并三唑、2-〔2-羟基-4-(3-甲基丙烯酰氧基丙基)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、辛基(3,5-二叔丁基-4-羟基)苯甲酸酯、十二烷基(3,5-二叔丁基-4-羟基)苯甲酸酯、十四烷基(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、十八烷基(3,5-二叔丁基-4-羟基)苯甲酸酯、山萮基(3,5-二叔丁基-4-羟基)苯甲酸酯等苯甲酸酯类;2-乙基-2’-乙氧基草酰苯胺、2-乙氧基-4’-十二烷基草酰苯胺等取代草酰苯胺类;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;各种金属盐、或金属螯合物、特别是镍、铬的盐、或螯合物类等。这些紫外线吸收剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的紫外线吸收剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.001~10质量份的量,更优选成为0.005~1质量份的量。
作为上述增塑剂,例如可以举出:邻苯二甲酸二丁酯、邻苯二甲酸丁基苄酯、邻苯二甲酸丁基己酯、邻苯二甲酸二庚酯、邻苯二甲酸二辛酯、双(2-乙基己基)邻苯二甲酸酯、邻苯二甲酸二异辛酯、邻苯二甲酸二异壬酯、邻苯二甲酸二异癸酯、邻苯二甲酸二月桂酯、邻苯二甲酸二环己酯、对苯二甲酸二辛酯、双(2-乙基己基)对苯二甲酸酯等苯二甲酸系增塑剂;己二酸二辛酯、双(2-乙基己基)己二酸酯、己二酸二异壬酯、己二酸二异癸酯、双(丁基二甘醇)己二酸酯等己二酸系增塑剂;磷酸三苯酯、磷酸三甲苯酯、三(二甲苯基)磷酸酯、三(异丙基苯基)磷酸酯、磷酸三乙酯、磷酸三丁酯、磷酸三辛酯、三(丁氧基乙基)磷酸酯、磷酸辛基二苯酯等磷酸酯系增塑剂;使用乙二醇、二乙二醇、三乙二醇、1,2-丙二醇、1,3-丙二醇、2-甲基-1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、三羟甲基丙烷等多元醇和草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、肉桂酸等二元酸,根据需要使用一元醇、单羧酸(乙酸、月桂酸、芳香族酸等)等作为阻聚剂的聚酯系增塑剂;环氧化大豆油、环氧化亚麻籽油、环氧化桐油、环氧化鱼油、环氧化牛脂油、环氧化蓖麻油、环氧化红花油、环氧化硬脂酸甲酯、环氧化硬脂酸丁酯、环氧化硬脂酸(2-乙基己基)酯、环氧化硬脂酸硬脂酯、环氧化聚丁二烯、三(环氧丙基)异氰脲酸酯、环氧化妥尔油脂肪酸酯、环氧化亚麻籽油脂肪酸酯、双酚A二缩水甘油醚、乙烯基环己烯二环氧化物、二环己烯二环氧化物、3,4-环氧环己基甲酯、环氧环己烷羧酸酯等环氧系增塑剂、以及四氢苯二甲酸系增塑剂、壬二酸系增塑剂、双(2-乙基己基)癸二酸酯、癸二酸二丁酯等癸二酸系增塑剂、硬脂酸系增塑剂、柠檬酸系增塑剂、偏苯三酸系增塑剂、均苯四酸系增塑剂、亚联苯基聚羧酸系增塑剂、三羟甲基丙烷三苯甲酸酯、二乙二醇二苯甲酸酯、二丙二醇二苯甲酸酯、(2-乙基己基)苯甲酸酯、异癸基苯甲酸酯等芳香族酸酯系增塑剂等。优选可以举出聚酯系增塑剂、苯二甲酸系增塑剂、偏苯三酸系增塑剂、己二酸系增塑剂、癸二酸系增塑剂、环氧系增塑剂。这些增塑剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的增塑剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为1~90质量份,更优选成为10~80质量份的量。
作为上述结晶成核剂,例如可以举出:苯甲酸钠、4-叔丁基苯甲酸铝盐、己二酸钠、双环[2.2.1]庚烷-2,3-二羧酸二钠等羧酸金属盐、双(4-叔丁基苯基)磷酸钠、2,2’-亚甲基双(4,6-二叔丁基苯基)磷酸钠、2,2’-亚甲基双(4,6-二叔丁基苯基)磷酸锂、双[2,2’-亚甲基双(4,6-二叔丁基苯基)磷酸]碱式铝等磷酸酯金属盐、二苄叉基山梨醇、双(甲基苄叉基)山梨醇、双(对乙基苄叉基)山梨醇、双(二甲基苄叉基)山梨醇、1,2,3-三脱氧-4,6:5,7-O-双(4-丙基苄叉基)壬醇等多元醇衍生物、N,N’,N”-三[2-甲基环己基]-1,2,3-丙烷三甲酰胺(RIKACLEAR PC1)、N,N’,N”-三环己基-1,3,5-苯三甲酰胺、N,N’-二环己基-萘二甲酰胺、1,3,5-三(二甲基异丙基氨基)苯等酰胺化合物等。这些结晶成核剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的结晶成核剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.001~10质量份的量,更优选成为0.01~5质量份的量。
作为上述本发明的磷酸盐系阻燃剂以外的阻燃剂,例如可以举出:磷酸三苯酯、磷酸三甲苯酯、三(二甲苯基)磷酸酯、磷酸甲苯基二苯酯、甲苯基-2,6-二(二甲苯基)磷酸酯、间苯二酚双(二苯基磷酸酯)、(1-甲基乙叉基)-4,1-亚苯基四苯基二磷酸酯、1,3-亚苯基四(2,6-二甲基苯基)磷酸酯、株式会社ADEKA制的商品名“ADK STAB FP-500”、“ADK STAB FP-600”、“ADK STAB FP-800”、“ADK STAB FP-900L”等芳香族磷酸酯、苯基膦酸二乙烯酯、苯基膦酸二烯丙酯、苯基膦酸(1-丁烯基)酯等膦酸酯、二苯基次膦酸苯酯、二苯基次膦酸甲酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物衍生物等次膦酸酯、双(2-烯丙基苯氧基)膦腈、二甲苯基膦腈等膦腈化合物、红磷等磷系阻燃剂、氢氧化镁、氢氧化铝等金属氢氧化物、溴化双酚A型环氧树脂、溴化苯酚酚醛清漆型环氧树脂、六溴苯、五溴甲苯、乙撑双(五溴苯基)、乙撑双四溴邻苯二甲酰亚胺、1,2-二溴-4-(1,2-二溴乙基)环己烷、四溴环辛烷、六溴环十二烷、双(三溴苯氧基)乙烷、溴化聚苯醚、溴化聚苯乙烯和2,4,6-三(三溴苯氧基)-1,3,5-三嗪、三溴苯基马来酰亚胺、三溴苯基丙烯酸酯、三溴苯基甲基丙烯酸酯、四溴双酚A型二甲基丙烯酸酯、五溴苄基丙烯酸酯、溴化苯乙烯等溴系阻燃剂等。这些阻燃剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的这些本发明的磷酸盐系阻燃剂以外的阻燃剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为1~90质量份的量,更优选成为3~80质量份的量。
对于上述阻燃助剂,作为无机系的阻燃助剂,例如可以举出氧化钛、氧化铝、氧化镁、水滑石、滑石、蒙脱石等无机化合物、和其表面处理品,例如可以举出TIPAQUE R-680(氧化钛:石原产业株式会社制)、Kyowamag 150(氧化镁: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)、ALCAMIZER 4(锌改性水滑石:协和化学工业株式会社制)等无机系的阻燃助剂。作为有机系的阻燃助剂,例如可以举出季戊四醇、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-羟基乙基)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、山梨醇、赤藓醇、木糖醇、木糖、蔗糖(sucrose)、海藻糖、肌醇、果糖、麦芽糖、乳糖等多元醇化合物。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和季戊四醇的缩合物的组中的1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。另外,也可以适合使用THEIC和山梨醇。这些阻燃助剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的阻燃助剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.01~20质量份的量,更优选成为0.1~10质量份的量。
作为上述防滴落剂,可以举出氟系防滴落剂、有机硅橡胶类、层状硅酸盐等。作为氟系防滴落剂,可以举出聚四氟乙烯、聚偏二氟乙烯、聚六氟丙烯等氟系树脂、全氟甲磺酸钠盐、全氟-正丁磺酸钾盐、全氟-叔丁磺酸钾盐、全氟辛磺酸钠盐、全氟-2-乙基己磺酸钙盐等全氟烷烃磺酸碱金属盐化合物或全氟烷烃磺酸碱土金属盐等。另外,作为层状硅酸盐,可以举出蒙脱石、皂石、锂蒙脱石、贝得石、硅镁石(stevensite)、绿脱石等膨润石系粘土矿物、蛭石、埃洛石、溶胀性云母、滑石等,也可以为在该层间嵌入有机阳离子、季铵阳离子、鏻阳离子而成者。这些防滴落剂可以单独使用1种,也可以并用2种以上而使用。防滴落剂中,从防滴落性的方面出发,特别优选氟系防滴落剂,最优选聚四氟乙烯。
本发明的阻燃剂组合物中的防滴落剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.005~5质量份的量,进一步优选成为0.01~5质量份的量,特别优选成为0.05~3质量份的量,最优选成为0.1~1质量份的量。防滴落剂的含量如果低于0.005质量份,则防滴落效果不充分,如果超过5质量份,则有时使树脂的特性降低。
作为上述丙烯酸类加工助剂,可以使用使(甲基)丙烯酸酯的1种聚合或使2种以上共聚而得到者。作为聚合或共聚的(甲基)丙烯酸酯的例子,可以举出丙烯酸甲酯、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、甲基丙烯酸十二烷酯、甲基丙烯酸十三烷酯等(甲基)丙烯酸酯等。另外,除上述以外,还可以举出(甲基)丙烯酸、含有羟基的(甲基)丙烯酸酯。
本发明的阻燃剂组合物中的丙烯酸类加工助剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.01~10质量份的量,更优选成为0.03~1质量份的量。
作为上述填充剂,例如可以举出滑石、云母、碳酸钙、氧化钙、氢氧化钙、碳酸镁、氢氧化镁、氧化镁、硫酸镁、氢氧化铝、硫酸钡、玻璃粉末、玻璃纤维、粘土、白云石、云母、二氧化硅、氧化铝、钛酸钾须晶、硅灰石、纤维状镁氧化硫酸盐等,可以适宜选择粒径(纤维状者中为纤维直径、纤维长度和长宽比)而使用。另外,填充剂可以使用根据需要进行了表面处理而成者。这些填充剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的填充剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.01~90质量份的量,更优选成为0.1~50质量份的量,进一步优选成为5~40质量份的量。
上述水滑石类例如是已知作为天然物、合成物的由镁、铝、羟基、碳酸基和任意结晶水形成的复合盐化合物,可以举出:将镁或铝的一部分用碱金属、锌等其他金属取代而成者、将羟基、碳酸基用其他阴离子基取代而成者。另外,可以为将结晶水进行了脱水而成者,也可以为用硬脂酸等高级脂肪酸、油酸碱金属盐等高级脂肪酸金属盐、十二烷基苯磺酸碱金属盐等有机磺酸金属盐、高级脂肪酸酰胺、高级脂肪酸酯或蜡等覆盖而成者。它们可以为天然物,而且也可以为合成品,可以不受限于晶体结构、晶粒等而使用。这些水滑石类可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的水滑石类的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.01~90质量份的量,更优选成为0.1~50质量份的量,进一步优选成为5~40质量份的量。
作为上述金属皂,例如可以举出锂、钠、镁、钙、铝、锌等金属与月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山萮酸、油酸、12-羟基硬脂酸等饱和或不饱和脂肪酸的盐。这些金属皂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的金属皂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.001~10质量份的量,更优选成为0.01~5质量份的量。
上述抗静电剂例如可以举出:脂肪酸季铵离子盐、多胺季盐等阳离子系抗静电剂;高级醇磷酸酯盐、高级醇EO加成物、聚乙二醇脂肪酸酯、阴离子型的烷基磺酸盐、高级醇硫酸酯盐、高级醇乙烯氧化物加成物硫酸酯盐、高级醇乙烯氧化物加成物磷酸酯盐等阴离子系抗静电剂;多元醇脂肪酸酯、聚二醇磷酸酯、聚氧乙烯烷基烯丙醚等非离子系抗静电剂;烷基二甲基氨基乙酸甜菜碱等两性型烷基甜菜碱、咪唑啉型两性活性剂等两性抗静电剂。这些抗静电剂可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的抗静电剂的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.01~20质量份的量,更优选成为0.03~10质量份的量。
作为上述颜料,也可以使用市售的颜料,例如可以举出颜料红1、2、3、9、10、17、22、23、31、38、41、48、49、88、90、97、112、119、122、123、144、149、166、168、169、170、171、177、179、180、184、185、192、200、202、209、215、216、217、220、223、224、226、227、228、240、254;颜料橙13、31、34、36、38、43、46、48、49、51、52、55、59、60、61、62、64、65、71;颜料黄1、3、12、13、14、16、17、20、24、55、60、73、81、83、86、93、95、97、98、100、109、110、113、114、117、120、125、126、127、129、137、138、139、147、148、150、151、152、153、154、166、168、175、180、185;颜料绿7、10、36;颜料蓝15、15:1、15:2、15:3、15:4、15:5、15:6、22、24、56、60、61、62、64;颜料紫1、19、23、27、29、30、32、37、40、50等。这些颜料可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的颜料的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.001~5质量份的量,更优选成为0.003~3质量份的量。
作为上述染料,例如可以举出偶氮染料、蒽醌染料、靛蓝染料、三芳基甲烷染料、呫吨染料、茜素染料、吖啶染料、茋染料、噻唑染料、萘酚染料、喹啉染料、硝基染料、茚满染料、恶嗪染料、酞菁染料、花青染料等。这些染料可以单独使用1种,也可以并用2种以上而使用。
本发明的阻燃剂组合物中的染料的含量可以设为不有损本发明的效果的范围,相对于含有本发明的阻燃剂组合物的阻燃性树脂组合物中所含的合成树脂100质量份,优选成为0.001~5质量份的量,更优选成为0.003~3质量份的量。
此外,本发明的阻燃剂组合物中,可以根据需要在不显著有损本发明的效果的范围内配混:通常合成树脂中使用的添加剂、例如交联剂、防雾剂、防渗出剂、表面处理剂、荧光剂、防霉剂、杀菌剂、发泡剂、金属减活剂、脱模剂、丙烯酸类加工助剂以外的加工助剂等。这些成分可以预先配混在本发明的阻燃剂组合物中,也可以在制备后述的阻燃性树脂组合物时配混。
为了得到本发明的阻燃剂组合物,只要将(A)成分和(B)成分与根据需要的其他任意成分进行混合即可,混合中可以使用各种混合机。混合时可以进行加热。如果列举能使用的混合机的例子,则可以举出转鼓混合机、亨舍尔混合机、螺带式混合机、V型混合机、W型混合机、超级混合机、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,优选配混在合成树脂中作为阻燃性树脂组合物使用。
<阻燃性树脂组合物>
本发明的阻燃性树脂组合物含有:合成树脂中的至少1种以上、和本发明的阻燃剂组合物中的至少1种以上。
本发明的阻燃性树脂组合物中的阻燃剂组合物的含量相对于合成树脂100质量份,优选10~400质量份、更优选10~300质量份、进一步优选10~100质量份、特别优选20~80质量份。阻燃剂组合物的含量相对于合成树脂100质量份如果少于10质量份,则有时无法发挥充分的阻燃性,如果多于400质量份,则有时有损树脂原本的物性。
作为上述合成树脂的具体例,可以举出: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、乙烯-丙烯共聚物、乙烯-丙烯-二烯三元共聚物、乙烯-乙酸乙烯酯共聚物、乙烯系离聚物、聚乙烯醇、乙烯-乙烯醇共聚物、氯化聚乙烯、氯磺化聚乙烯等烯烃系树脂;聚氯乙烯、聚偏二氯乙烯、氯化聚乙烯、氯化聚丙烯、聚偏二氟乙烯、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-偏二氯乙烯共聚物、氯乙烯-偏二氯乙烯-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;聚苯乙烯、苯乙烯-丁二烯共聚物、苯乙烯-丁二烯-苯乙烯·嵌段共聚物(SBS)、苯乙烯-乙烯-丁烯-苯乙烯·嵌段共聚物(SEBS)、丙烯腈-苯乙烯共聚物(AS)、丙烯腈-丁二烯-苯乙烯共聚物(ABS)、丙烯腈-氯化聚乙烯-苯乙烯共聚物(ACS)、甲基丙烯酸甲酯-丁二烯-苯乙烯共聚物(MBS)等苯乙烯系树脂;聚丙烯酸丁酯、丙烯酸酯-丙烯腈共聚物、聚甲基丙烯酸甲酯等丙烯酸系或甲基丙烯酸系树脂;乙烯-乙酸乙烯酯共聚物、聚乙酸乙烯酯等乙酸乙烯酯系树脂;聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚环己烷二亚甲基对苯二甲酸酯、聚萘二甲酸乙二醇酯、聚萘二甲酸丁二醇酯等芳香族酯系树脂;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、聚苹果酸、聚乙醇酸、聚二氧杂环己烷、聚(2-氧杂环丁烷酮)等降解性脂肪族酯系树脂;聚酰胺6、聚酰胺66、聚酰胺11、聚酰胺12、芳香族聚酰胺、聚酰亚胺等聚酰胺系或聚酰亚胺系树脂;聚苯氧化物、聚碳酸酯、聚碳酸酯/ABS树脂、支链聚碳酸酯、聚缩醛、聚苯硫醚、聚氨酯、纤维素系树脂、聚砜、聚苯醚、聚醚酮、聚醚醚酮、聚乙烯醇缩甲醛、聚乙烯醇缩丁醛、石油树脂、香豆酮树脂、液晶聚合物等热塑性树脂和它们的共混物。
另外,上述合成树脂可以为异戊二烯橡胶、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、有机硅橡胶、聚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弹性体。
本发明中,这些合成树脂可以单独使用,也可以组合2种以上而使用。另外,上述合成树脂也可以进行合金化。
这些合成树脂可以无论分子量、聚合度、密度、软化点、不溶组分对溶剂的比例、立构规整性的程度、催化剂残渣的有无、成为原料的单体的种类、配混比率、聚合催化剂的种类(例如齐格勒型催化剂、茂金属催化剂等)等而使用。这些合成树脂中,从能赋予优异的阻燃性的方面出发,优选选自由烯烃系树脂、苯乙烯系树脂、乙酸乙烯酯系树脂和它们的共聚物组成的组中的1种以上,也优选并用它们与热塑性弹性体的情况。
本发明的阻燃剂组合物对树脂的配混方法没有特别限定,可以采用公知的方法。作为具体的配混方法,可以举出如下方法:在通常的搅拌机、混合机等中进行混合的方法;在挤出机等中进行熔融混炼的方法;与溶剂一起进行混合并进行溶液流延的方法等。
<成型体>
本发明的成型体通过将本发明的阻燃性树脂组合物、优选使用了热塑性树脂的阻燃性树脂组合物进行成型而得到。对于成型方法和成型条件没有特别限制,可以使用公知的成型方法和成型条件。作为具体的成型方法,可以举出挤出加工、压延加工、注射成型、辊、压缩成型、吹塑成型、旋转成型等,可以制造树脂板、片、薄膜、瓶、纤维、异形品等各种形状的成型体。
本发明的阻燃性树脂组合物和其成型体可以用于电气/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、建筑材料、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、文字处理器、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、电子记事本、卡、支架、文具等办公室、OA设备、洗衣机、冰箱、吸尘器、微波炉、照明器具、游戏机、熨斗、被炉等家电设备、TV、VTR、摄像机、收录两用机、磁带录音机、迷你光盘、CD播放器、扬声器、液晶显示器等AV设备、连接器、继电器、电容器、开关、印刷电路板、线圈骨架、半导体密封材料、LED密封材料、电线、电缆、变压器、偏转线圈、配电板、时钟等电气/电子部件和通信设备、OA设备等的壳体(框、壳体、盖、外饰)、部件、汽车内外饰材料的用途。
此外,本发明的阻燃性树脂组合物和其成型体可以用于座位(填充物、外层材料等)、带、天花板内饰、敞篷车顶、扶手、门饰、后行李托盘、地毯、垫、防晒遮阳板、轮罩、床垫套、安全气囊、绝缘材料、肩带、挂绳带、电线覆盖材料、电气绝缘材料、涂料、涂覆材料、覆盖材料、地板材料、墙角壁、地毯、壁纸、墙布、外饰材料、内饰材料、屋顶材料、甲板材料、墙材料、柱材、底板、围墙材料、骨架和模具、门窗型材、薄木板、木板墙、天台、阳台、隔音板、隔热板、窗材料等汽车、混合动力汽车、电动汽车、车辆、船舶、航空机、建筑物、住宅和建筑用材料或土木材料,衣料、窗帘、床单、胶合板、合成纤维板、地毯、门垫、床单、水桶、软管、容器、眼镜、包、箱子、护目镜、滑雪板、球拍、帐篷、乐器等生活用品、运动用品等各种用途。
实施例
以下,根据实施例和比较例具体示出本发明。以下的实施例所示的材料、物质、配混量、其比例和操作等只要不脱离本发明的主旨就可以适宜变更。因此,本发明不受以下的实施例的任何限制。需要说明的是,以下的实施例中,只要没有特别记载,成分的配混量就是质量基准。
<(A)成分:磷酸盐系阻燃剂的制造>
以以下的制造例所示的方法制造作为(A)成分的构成成分的(A-1)成分和(A-2)成分。需要说明的是,以下的制造例1、2中,纯度使用离子色谱测定装置ICS-2100(ThermoFisher Scientific Co.,Ltd.制)、Dionex IonPac AS-19柱(Thermo Fisher ScientificCo.,Ltd.制)、和电导率检测器而测定。
〔制造例1〕
(A-1)成分:三聚氰胺盐
使正磷酸三聚氰胺以220℃以固相状态进行加热缩合反应6小时,制造以焦磷酸三聚氰胺为主成分的三聚氰胺盐。三聚氰胺盐不经纯化而直接使用。三聚氰胺盐中的焦磷酸三聚氰胺的纯度为98.5%。
〔制造例2〕
(A-2)成分:哌嗪盐
使二磷酸哌嗪以250℃以固相状态进行加热缩合反应1小时,制造以焦磷酸哌嗪为主成分的哌嗪盐。哌嗪盐不经纯化而直接使用。哌嗪盐中的焦磷酸哌嗪的纯度为99.0%。
<试验片制作条件>
使用双螺杆挤出机(株式会社日本制钢所制TEX25αIII),在220℃、10kg/小时的加工条件下将基于下述的表1~7所示的配混量共混而成的树脂组合物造粒,得到粒料。使用卧式注射成型机(日精树脂工业株式会社制NEX80),在树脂温度220℃、模具温度40℃的加工条件下,将得到的粒料成型,制作阻燃性评价用试验片(127mm×12.7mm×1.6mm)和夏比冲击强度测定用试验片(80mm×10mm×4mm)。使用这些试验片,依据下述的评价方法,实施UL-94V阻燃性、耐水性和夏比冲击强度的各评价。基于各评价试验的结果,分别示于下述的表1~7。
<阻燃性UL-94V评价方法>
将试验片(127mm×12.7mm×1.6mm)成型后,立即在23℃、湿度50%RH的恒温恒湿槽内静置7天,依据UL-94V标准,划分燃烧等级。燃烧等级为V-0是最高,随着成为V-1、V-2而阻燃性降低。其中,将均不属于V-0~V-2等级者记作NR(No Rating)。
<耐水性试验方法(1)>
将试验片(80mm×10mm×4mm)成型后,立即在23℃、湿度50%RH的恒温恒湿槽内静置7天。使该试验片13条浸渍于240mL的超纯水中,在70℃下静置7天后,取出试验片。使用Hanna制EC试验机/HI98303N(DiST3)测定浸渍后的水的电导率(μS/cm)。另外,将未放入(B)成分的配方(比较例1-1、2-1、3-1)作为基准,将以比例表示试验片浸渍后的水的电导率的增减的数值作为水溶性成分的溶出量的抑制效果(表中,记作“溶出抑制效果(70℃)”)。该数值为负值的情况下,表示与成为基准的比较例相比,试验片浸渍后的水的电导率小、水溶性成分的溶出量被抑制。
<耐水性试验方法(2)>
将试验片(127mm×12.7mm×1.6mm)成型后,立即在23℃、湿度50%RH的恒温恒湿槽内静置7天后,在减压下、以70℃干燥24小时。使该试验片2张浸渍于93mL的超纯水中,在85℃下静置7天后,取出试验片。使用Hanna制EC试验机/HI98303N(DiST3)测定浸渍后的水的电导率(μS/cm)。另外,将未放入(B)成分的配方(比较例3-1、4-1、5-1)作为基准,将以比例表示试验片浸渍后的水的电导率的增减的数值作为水溶性成分的溶出量的抑制效果(表中,记作“溶出抑制效果(85℃)”)。该数值为负值的情况下,表示与成为基准的比较例相比,试验片浸渍后的水的电导率减少,成分的溶出量被抑制。
<夏比冲击强度评价方法>
将得到的试验片(80mm×10mm×4mm)成型后,立即在23℃、湿度50%RH的恒温恒湿槽内静置7天,在试验片上制作切口。从恒温恒湿槽中取出试验片,依据JIS K7111迅速测定夏比冲击强度(kJ/m2)。
需要说明的是,表1~7中的各成分的详细情况如下所述。
ICP:抗冲共聚物聚丙烯(商品名Prime Polypro J-754HP、Prime Polymer Co.,Ltd.制、熔体流动速率=14g/10分钟)
LDPE:低密度聚乙烯(商品名NOVATEC LF441B、日本聚乙烯(株)制、熔体流动速率=2.0g/10分钟)
EVA:乙烯-乙酸乙烯酯共聚物(商品名Ultrasen 635、东曹株式会社制、熔体流动速率=2.0g/10分钟、乙酸乙烯酯含有率=25%)
PP:聚丙烯(商品名NOVATEC FY4、Japan Polypropylene Corporation制、熔体流动速率=5.0g/10分钟)
SEBS:苯乙烯-乙烯-丁烯-苯乙烯·嵌段共聚物(商品名Tuftec H1062、旭化成株式会社制、熔体流动速率=4.5g/10分钟)
酚系抗氧化剂:四[3-(3,5-二叔丁基-4-羟基苯基)丙酰氧基甲基]甲烷磷系抗氧化剂:三(2,4-二叔丁基苯基)亚磷酸酯
中和剂:硬脂酸钙
结晶成核剂:2,2’-亚甲基双(4,6-二叔丁基苯基)磷酸钠
填充剂:滑石
三聚氰胺盐:制造例1中制造的三聚氰胺盐
哌嗪盐:制造例2中制造的哌嗪盐
铵盐:多磷酸铵(商品名Exolit AP422、Clariant公司制)
马来酸酐改性聚乙烯(1):商品名OREVAC 18302N、Arkema公司制、熔体流动速率=1.5g/10分钟、酸值=9mgKOH/g、质均分子量(Mw)=125000
马来酸酐改性聚乙烯(2):商品名OREVAC OE808、Arkema公司制、熔体流动速率=0.6g/10分钟、质均分子量(Mw)=208000
马来酸酐改性聚丙烯:商品名UMEX1010、三洋化成工业株式会社制、酸值=52mgKOH/g、质均分子量(Mw)=30000
氧化锌:商品名氧化锌1种、三井金属矿业株式会社制
聚碳二亚胺:商品名CARBODILITE LA-1、Nisshinbo Chemical Inc.制硅油:商品名KF-96、信越化学株式会社制
环氧系偶联剂:2-(3,4-环氧环己基)乙基三甲氧基硅烷、商品名Silaace S530、CHISSO CORPORATION制
润滑剂:甘油单硬脂酸酯、商品名RIKEMAL S-100、Riken Vitamin Co.,Ltd.制
[表1]
[表2]
[表3]
[表4]
[表5]
[表6]
[表7]
通过实施例1-1~1-14与比较例1-1~1-6的比较、实施例2-1~2-4与比较例2-1的比较、和实施例3-1~3-3与比较例3-1~3-2的比较,可知:在抗冲共聚物聚丙烯中并用了本发明的(A)成分和(B)成分的树脂组合物与未配混(B)成分者、配混聚碳二亚胺代替(B)成分者相比,耐水试验后的浸渍水的电导率小,耐水性优异,夏比冲击强度进一步改善。
比较例1-1~1-5中,可知:根据聚碳二亚胺的增量而UL-94V燃烧等级降低至V-2水平,阻燃性能降低。另一方面,可知:实施例1-1~1-5中,增量本发明的(B)成分至15质量份,UL-94V燃烧等级也维持V-1以上。
比较例3-1中,耐水性试验后的UL-94V燃烧等级降低至V-2,但实施例3-1~3-3中,耐水性试验后的UL-94V燃烧等级未降低。
根据实施例4-1~4-2与比较例4-1~4-2的比较、和实施例5-1~5-2与比较例5-1~5-2的比较,基础树脂为LDPE/EVA、PP/SEBS的情况下,并用了本发明的(A)成分和(B)成分的树脂组合物也示出耐水性优异的结果而不降低阻燃性。
Claims (11)
1.一种阻燃剂组合物,其特征在于,含有下述(A)成分和下述(B)成分,
(A)成分:含有下述(A-1)~(A-3)成分中的至少任一者的磷酸盐系阻燃剂
(A-1)成分:选自由正磷酸三聚氰胺、焦磷酸三聚氰胺和多磷酸三聚氰胺组成的组中的1种以上的三聚氰胺盐
(A-2)成分:选自由正磷酸哌嗪、焦磷酸哌嗪和多磷酸哌嗪组成的组中的1种以上的哌嗪盐
(A-3)成分:选自由正磷酸铵、焦磷酸铵和多磷酸铵组成的组中的1种以上的铵盐;
(B)成分:酸改性聚烯烃中的1种以上。
2.根据权利要求1所述的阻燃剂组合物,其中,相对于所述(A)成分100质量份,含有所述(B)成分0.5~75质量份。
3.根据权利要求1所述的阻燃剂组合物,其中,所述(B)成分为选自马来酸改性聚烯烃和马来酸酐改性聚烯烃中的1种以上。
4.根据权利要求1所述的阻燃剂组合物,其中,所述(B)成分的酸改性聚烯烃的酸值为1~100mgKOH/g。
5.根据权利要求1所述的阻燃剂组合物,其中,所述(B)成分的酸改性聚烯烃的质均分子量以聚苯乙烯换算计为1000~500000。
6.根据权利要求1所述的阻燃剂组合物,其中,还含有选自由硅油、环氧系偶联剂和润滑剂组成的组中的至少1种作为(C)成分。
7.根据权利要求1所述的阻燃剂组合物,其中,还含有氧化锌作为(D)成分。
8.一种阻燃性树脂组合物,其特征在于,在合成树脂中含有权利要求1所述的阻燃剂组合物。
9.根据权利要求8所述的阻燃性树脂组合物,其中,相对于所述合成树脂100质量份,含有所述阻燃剂组合物10~400质量份。
10.根据权利要求8所述的阻燃性树脂组合物,其中,所述合成树脂为选自由烯烃系树脂、苯乙烯系树脂、乙酸乙烯酯系树脂和它们的共聚物组成的组中的1种以上。
11.一种成型体,其特征在于,其是由权利要求8所述的阻燃性树脂组合物得到的。
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CN117534915A (zh) * | 2024-01-09 | 2024-02-09 | 广东电缆厂有限公司 | 一种无卤低烟阻燃电缆护套及其制备方法和包含该护套的电缆 |
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CN117534915B (zh) * | 2024-01-09 | 2024-03-22 | 广东电缆厂有限公司 | 一种无卤低烟阻燃电缆护套及其制备方法和包含该护套的电缆 |
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