CN113574114B - 红外线屏蔽透明构件用树脂组合物和成型品 - Google Patents
红外线屏蔽透明构件用树脂组合物和成型品 Download PDFInfo
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- CN113574114B CN113574114B CN202080019964.4A CN202080019964A CN113574114B CN 113574114 B CN113574114 B CN 113574114B CN 202080019964 A CN202080019964 A CN 202080019964A CN 113574114 B CN113574114 B CN 113574114B
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Abstract
本发明提供一种在保持高的透明性的同时具有耐湿热性良好的红外线屏蔽性能的树脂组合物。本发明的树脂组合物的特征在于,相对于(A)聚碳酸酯树脂(A成分)100重量份,含有(B)通式MxWyOz(其中,M为选自H、He、碱金属、碱土金属、稀土元素、Mg、Zr、Cr、Mn、Fe、Ru、Co、Rh、Ir、Ni、Pd、Pt、Cu、Ag、Au、Zn、Cd、Al、Ga、In、Tl、Si、Ge、Sn、Pb、Sb、B、F、P、S、Se、Br、Te、Ti、Nb、V、Mo、Ta、Re、Be、Hf、Os、Bi、I中的1种以上的元素,W为钨,O为氧,0.001≤x/y≤1,2.2≤z/y≤3.0)表示的复合钨氧化物微粒(B成分)0.0001~0.2重量份、(C)环氧树脂(C成分)0.0001~0.1重量份以及(D)作为以由脂肪酸和多元醇构成的全酯为主成分的脂肪酸酯的脱模剂(D成分)0.001~0.5重量份。
Description
技术领域
本发明涉及作为具有红外线吸收性能的无机材料的含有复合钨氧化物微粒的聚碳酸酯树脂组合物、以及由该聚碳酸酯树脂组合物构成的成型品。
背景技术
具有红外线屏蔽性能的透明材料具有抑制室内的温度上升、抑制人的体感温度上升的效果,通过用于汽车用途、建材用途等的窗构件而期待环境负荷减少的效果。特别是,通过对透明树脂赋予红外线屏蔽性能,从轻型化和热管理的观点出发,抑制CO2排出量等减少环境负荷的效果大。作为体现红外线屏蔽性能的手法,专利文献1中公开了对透明树脂赋予复合钨氧化物微粒的技术,但存在湿热条件下红外线屏蔽性能经时劣化的问题。专利文献2中公开了通过限定复合钨氧化物微粒的粒径而提高耐湿热性的技术,但其效果不充分。另外,专利文献3中公开了配合脂肪酸酯而提高树脂的热稳定性的技术,但看不到提高红外线屏蔽性能的耐湿热性的效果。另外,专利文献4中公开了通过在透明树脂中配合环氧树脂而抑制树脂的水解的技术,但看不到提高红外线屏蔽性能的耐湿热性的效果。因此,要求赋予复合钨氧化物微粒的透明树脂的红外线屏蔽性能的耐湿热性的提高。
现有技术文献
专利文献
专利文献1:日本特许第5714826号公报
专利文献2:日本特开2017-95686号公报
专利文献3:日本特开2008-156386号公报
专利文献4:日本特表2003-531926号公报
发明内容
本发明的目的是得到在保持高的透明性的同时具有耐湿热性良好的红外线屏蔽性能的树脂组合物及其成型品。
本发明人等为了解决上述课题进行了深入研究,结果发现,通过在聚碳酸酯树脂中添加复合钨氧化物微粒、环氧树脂以及脂肪酸酯,得到耐湿热性优异且显示高的红外线屏蔽性能和高的透过性的聚碳酸酯树脂组合物和由其形成的成型品。即,上述课题通过如下树脂组合物实现,该树脂组合物中,相对于(A)聚碳酸酯树脂(A成分)100重量份,含有(B)通式MxWyOz(其中,M为选自H、He、碱金属、碱土金属、稀土元素、Mg、Zr、Cr、Mn、Fe、Ru、Co、Rh、Ir、Ni、Pd、Pt、Cu、Ag、Au、Zn、Cd、Al、Ga、In、Tl、Si、Ge、Sn、Pb、Sb、B、F、P、S、Se、Br、Te、Ti、Nb、V、Mo、Ta、Re、Be、Hf、Os、Bi、I中的1种以上的元素、W为钨、O为氧、0.001≤x/y≤1、2.2≤z/y≤3.0)表示的复合钨氧化物微粒(B成分)0.0001~0.2重量份、(C)环氧树脂(C成分)0.0001~0.1重量份以及(D)作为以由脂肪酸和多元醇构成的全酯为主成分的脂肪酸酯的脱模剂(D成分)0.001~0.5重量份。
本发明的树脂组合物在保持高的透明性的同时具有耐湿热性良好的红外线屏蔽性能,因此适于车辆用灯具、车辆用传感器罩、车辆用显示装置罩、车辆用窗构件、继电器用显示装置罩或者建筑材料用窗构件等,其在工业上所能起到的效果显著。
具体实施方式
以下,对本发明的各构成成分的详细进行说明。
(A成分:聚碳酸酯树脂)
本发明中作为A成分使用的聚碳酸酯树脂是使二元酚和碳酸酯前体反应而得到的。作为反应方法的一个例子,可以举出界面聚合法、熔融酯交换法、碳酸酯预聚物的固相酯交换法以及环状碳酸酯化合物的开环聚合法等。
作为这里使用的二元酚的代表性的例子,可举出对苯二酚、间苯二酚、4,4’-双酚、1,1-双(4-羟基苯基)乙烷、2,2-双(4-羟基苯基)丙烷(通称双酚A)、2,2-双(4-羟基-3-甲基苯基)丙烷、2,2-双(4-羟基苯基)丁烷、1,1-双(4-羟基苯基)-1-苯基乙烷、1,1-双(4-羟基苯基)环己烷、1,1-双(4-羟基苯基)-3,3,5-三甲基环己烷、2,2-双(4-羟基苯基)戊烷、4,4’-(对亚苯基二异亚丙基)二酚、4,4’-(间亚苯基二异亚丙基)二酚、1,1-双(4-羟基苯基)-4-异丙基环己烷、双(4-羟基苯基)氧化物、双(4-羟基苯基)硫化物、双(4-羟基苯基)亚砜、双(4-羟基苯基)砜、双(4-羟基苯基)酮、双(4-羟基苯基)酯、2,2-双(3,5-二溴-4-羟基苯基)丙烷、双(3,5-二溴-4-羟基苯基)砜、双(4-羟基-3-甲基苯基)硫化物、9,9-双(4-羟基苯基)芴以及9,9-双(4-羟基-3-甲基苯基)芴等。优选的二元酚为双(4-羟基苯基)烷烃,其中,从耐冲击性方面考虑,特别优选双酚A。
作为碳酸酯前体,可使用碳酰卤化物、碳酸二酯或者卤甲酸酯等,具体而言,可举出光气、碳酸二苯酯或者二元酚的二卤甲酸酯等。
通过将上述二元酚与碳酸酯前体利用界面聚合法制造聚碳酸酯树脂时,根据需要可以使用催化剂、末端停止剂、防止二元酚氧化的抗氧化剂等。另外,本发明的聚碳酸酯树脂包括将三官能以上的多官能性芳香族化合物共聚而得的支化聚碳酸酯树脂、将芳香族或者脂肪族(包括脂环族)的二官能性羧酸共聚而得的聚酯碳酸酯树脂、将二官能性醇(包括脂环族)共聚而得的共聚聚碳酸酯树脂、以及将上述二官能性羧酸和二官能性醇一起进行共聚而得的聚酯碳酸酯树脂。另外,也可以是将得到的聚碳酸酯树脂的2种以上混合而成的混合物。
作为三官能以上的多官能性芳香族化合物,可以使用1,1,1-三(4-羟基苯基)乙烷、1,1,1-三(3,5-二甲基-4-羟基苯基)乙烷等。
含有产生支化聚碳酸酯的多官能性化合物的情况下,上述的量在芳香族聚碳酸酯全量中为0.001~1摩尔%,优选为0.005~0.9摩尔%,特别优选为0.01~0.8摩尔%。另外,特别是熔融酯交换法的情况下,作为副反应,有时产生支链结构,但上述支链结构量也优选在芳香族聚碳酸酯总量中为0.001~1摩尔%,优选为0.005~0.9摩尔%,特别优选为0.01~0.8摩尔%。应予说明,上述比例可以通过1H-NMR测定来计算。
脂肪族的二官能性的羧酸优选α,ω-二羧酸。作为脂肪族的二官能性的羧酸,例如优选举出癸二酸(decanedic acid)、十二烷二酸、十四烷二酸、十八烷二酸、二十烷二酸等直链饱和脂肪族二羧酸,以及环己烷二羧酸等脂环族二羧酸。作为二官能性醇,更优选脂环族二醇,例如可例示环己烷二甲醇、环己烷二醇以及三环癸烷二甲醇等。
还可以使用将聚有机硅氧烷单位共聚而得的聚碳酸酯-聚有机硅氧烷共聚物。
界面聚合法的反应通常是二元酚与光气的反应,在酸结合剂和有机溶剂的存在下进行反应。作为酸结合剂,例如使用氢氧化钠、氢氧化钾等碱金属氢氧化物、吡啶等。
作为有机溶剂,例如可使用二氯甲烷、氯苯等卤代烃。
另外,为了促进反应,例如可以使用叔胺、季铵盐等催化剂,作为分子量调节剂,例如优选使用苯酚、对叔丁基苯酚、对枯基苯酚等单官能酚类。此外,作为单官能酚类,可以举出癸基苯酚、十二烷基苯酚、十四烷基苯酚、十六烷基苯酚、十八烷基苯酚、二十烷基苯酚、二十二烷基苯酚以及三十烷基苯酚等。这些具有较长链烷基的单官能酚类在要求提高流动性、耐水解性的情况下有效。
优选:反应温度通常为0~40℃,反应时间为数分钟~5小时,反应中的pH通常保持在10以上。
熔融法的反应通常是二元酚与碳酸二酯的酯交换反应,在非活性气体的存在下将二元酚和碳酸二酯混合,减压下通常在120~350℃进行反应。减压度是阶段性改变的,最终达到133Pa以下,使生成的酚类除去到体系外。反应时间通常为1~4小时左右。
作为碳酸二酯,例如可举出碳酸二苯酯、碳酸二萘酯、碳酸双(二苯基)酯、碳酸二甲酯、碳酸二乙酯以及碳酸二丁酯等,其中优选碳酸二苯酯。
为了加快聚合速度,可以使用聚合催化剂,作为聚合催化剂,例如可举出氢氧化钠、氢氧化钾等碱金属、碱土金属的氢氧化物、硼或铝的氢氧化物、碱金属盐、碱土金属盐、季铵盐、碱金属、碱土金属的醇盐、碱金属、碱土金属的有机酸盐、锌化合物、硼化合物、硅化合物、锗化合物、有机锡化合物、铅化合物、锑化合物、锰化合物、钛化合物、锆化合物等通常酯化反应、酯交换反应中使用的催化剂。催化剂可以单独使用,也可以并用2种以上使用。这些聚合催化剂的使用量相对于原料的二元酚1摩尔,优选在1×10-9~1×10-5当量,更优选在1×10-8~5×10-6当量的范围选择。
另外,聚合反应中,为了减少酚性的末端基,可以在聚缩合反应的后期或者结束后加入例如2-氯苯基苯基碳酸酯、2-甲氧基羰基苯基苯基碳酸酯以及2-乙氧基羰基苯基苯基碳酸酯等化合物。
进而,在熔融酯交换法中优选使用中和催化剂的活性的失活剂。作为上述失活剂的量,优选相对于残存的催化剂1摩尔使用0.5~50摩尔的比例。另外,相对于聚合后的芳香族聚碳酸酯以0.01~500ppm的比例,更优选以0.01~300ppm,特别优选以0.01~100ppm的比例使用。作为失活剂,优选举出十二烷基苯磺酸四丁基盐等/>盐,四乙基十二烷基苄基硫酸铵等铵盐等。上述以外的反应形式的详细在书籍和专利公报等中,是公知的。
聚碳酸酯树脂的粘度平均分子量优选14000~100000,更优选20000~30000,进一步优选22000~28000,特别优选23000~26000。超出上述范围而分子量过低的情况下,对硬涂剂的耐性容易变得不充分,超出上述范围而分子量过高的情况下,注塑成型变得困难,容易产生成型品的破裂、不均匀的阴影。在上述的优选的范围内,对硬涂剂的耐性充分的分子量下,本发明的树脂组合物能够减少由树脂流动的紊乱引起的成型品的不均匀的阴影,能够形成具有硬涂层的良好的聚碳酸酯树脂成型体。更优选的范围下,耐冲击性和成型加工性都优异。应予说明,上述聚碳酸酯树脂可以通过混合其粘均分子量在上述范围外的聚碳酸酯树脂而得到。
聚碳酸酯树脂的粘均分子量(M)由在二氯甲烷100ml中溶解了聚碳酸酯树脂0.7g的溶液在20℃求出的比粘度(ηsp)代入下式而求出。
ηsp/c=[η]+0.45×[η]2c(其中,[η]为极限粘度)
[η]=1.23×10-4M0.83
c=0.7
作为本发明中的聚碳酸酯树脂的形态,可以举出以下形态。即,可以使用由粘均分子量70000~300000的芳香族聚碳酸酯(PC-i)和粘均分子量10000~30000的芳香族聚碳酸酯(PC-ii)构成,且其粘均分子量为15000~40000、优选为20000~30000的芳香族聚碳酸酯(以下,有时称为“含有高分子量成分的芳香族聚碳酸酯”)。
上述含有高分子量成分的芳香族聚碳酸酯因PC-i的存在而增大聚合物的熵弹性,在本发明中优选的注射加压成型时更为有利。例如能够进一步减少滞留痕等外观不良,对应地可以扩大注射加压成型的条件宽度。另一方面,PC-ii成分的低分子量成分可以降低整体的熔融粘度,促进树脂的缓和,能够实现更低应变的成型。应予说明,使用含有支化成分的聚碳酸酯树脂也能看到相同的效果。
(B成分:复合钨氧化物微粒)
复合钨氧化物微粒(B成分)由通式MxWyOz表示。式中M表示选自H、He、碱金属、碱土金属、稀土元素、Mg、Zr、Cr、Mn、Fe、Ru、Co、Rh、Ir、Ni、Pd、Pt、Cu、Ag、Au、Zn、Cd、Al、Ga、In、Tl、Si、Ge、Sn、Pb、Sb、B、F、P、S、Se、Br、Te、Ti、Nb、V、Mo、Ta、Re、Be、Hf、Os、Bi、I中的1种以上的元素,优选为选自Li、Na、K、Rb、Cs、Mg、Ca、Sr以及Ba中的1种以上的元素,更优选为K、Rb或者Cs。另外,W表示钨,O表示氧。
x、y、z是满足0.001≤x/y≤1,2.2≤z/y≤3.0的式子的数。并且,x/y、z/y的范围分别优选0.01≤x/y≤0.5、2.7≤z/y≤3.0,更优选0.2≤x/y≤0.4、2.8≤z/y≤3.0。
复合钨氧化物微粒(B成分)的粒径优选1nm~800nm,更优选1nm~600nm,进一步优选1nm~300nm。粒径小于1nm时,凝聚效果增大,容易产生分散性不良,如果大于800nm,则有时产生透明树脂成型品的浑浊度变高等不良。
复合钨氧化物微粒(B成分)可以将作为起始原料的钨化合物在非活性气体气氛或还原性气体气氛中进行热处理而得到。经由该热处理得到的复合钨氧化物微粒具有充分的近红外线屏蔽力,具有作为红外线屏蔽微粒优选的性质。
复合钨氧化物微粒(B成分)的起始原料是以元素单质或者化合物的形式含有元素M的钨化合物。具体而言,优选为选自以元素单质或者化合物的形式含有元素M的三氧化钨粉末、二氧化钨粉末、钨氧化物的水合物、六氯化钨粉末、钨酸铵粉末、使六氯化钨溶解在醇中后干燥得到的钨氧化物的水合物粉末、使六氯化钨溶解在醇中后添加水使其沉淀将其干燥得到的钨氧化物的水合物粉末、将钨酸铵水溶液干燥得到的钨化合物粉末、以及金属钨粉末中的1种以上。应予说明,起始原料为溶液时,从各元素能够容易且均匀混合的观点出发,进一步优选使用钨酸铵水溶液、六氯化钨溶液。使用这些原料,将其在非活性气体气氛或还原性气体气氛中进行热处理,能够得到上述的复合钨氧化物微粒。
这里,为了制造作为各成分以分子等级均匀混合的起始原料的钨化合物,优选将各原料在溶液中混合,优选含有元素M的钨化合物能够溶解在水、有机溶剂等溶剂中。例如,可举出含有元素M的钨酸盐、氯化物盐、硝酸盐、硫酸盐、草酸盐、氧化物、碳酸盐、氢氧化物等,不限于这些,只要为溶液状态,就是优选的。
对于用于制造复合钨氧化物微粒(B成分)的原料,以下,再次详细进行说明。
用于得到通式MxWyOz表示的复合钨氧化物微粒(B成分)的起始原料可以使用混合了钨氧化物系粉末和上述M元素系粉末的粉末。作为钨氧化物系粉末,可举出三氧化钨粉末、二氧化钨粉末、钨氧化物的水合物、六氯化钨粉末、钨酸铵粉末、使六氯化钨溶解在醇中后干燥得到的钨氧化物的水合物粉末、使六氯化钨溶解在醇中后添加水使其沉淀、干燥得到的钨氧化物的水合物粉末、将钨酸铵水溶液干燥得到的钨化合物粉末、金属钨粉末等。另外,作为M元素系粉末,可举出含有M元素的单体或者化合物的粉末等。并且,作为用于得到复合钨氧化物微粒(B成分)的起始原料的钨化合物未溶液或者分散液时,各元素能够容易且均匀混合。从该观点出发,复合钨氧化物微粒(B成分)的起始原料进一步优选将六氯化钨的醇溶液或者钨酸铵水溶液和含有上述M元素的化合物的溶液混合后干燥而得的粉末。同样,复合钨氧化物的微粒(B成分)的起始原料优选为将使六氯化钨溶解在醇中后添加水而生成沉淀的分散液、和含有上述M元素的单体或者化合物的粉末或者含有上述M元素的化合物的溶液混合后干燥而得的粉末。
作为含有上述M元素的化合物,可举出M元素的钨酸盐、氯化物盐、硝酸盐、硫酸盐、草酸盐、氧化物、碳酸盐、氢氧化物等,不限于这些,只要为溶液状态即可。并且,工业上制造复合钨氧化物微粒(B成分)的情况下,使用钨氧化物的水合物粉末、三氧化钨和M元素的碳酸盐或氢氧化物时,在热处理等阶段不会产生有害的气体等,是理想的制造法。
这里,作为复合钨氧化物微粒(B成分)的非活性气氛中的热处理条件,优选650℃以上。在650℃以上经热处理的起始原料具有充分的近红外线屏蔽力,作为红外线屏蔽微粒是有效的。作为非活性气体,可以使用Ar、N2等非活性气体。
另外,作为还原性气氛中的热处理条件,优选首先将起始原料在还原性气体气氛中在100℃~850℃进行热处理,接着在非活性气体气氛中以650℃~1200℃的温度进行热处理。此时的还原性气体没有特别限定,但优选H2。另外,使用H2作为还原性气体时,作为还原气氛的组成,H2以体积比计可以优选0.1%以上,进一步优选2%以上。H2只要以体积比计为0.1%以上,就能够高效地还原。
从提高耐久性的观点出发,复合钨氧化物的微粒(B成分)的表面优选被含有Si、Ti、Zr、Al中的一种以上的金属的氧化物覆盖。覆盖方法没有特别限定,可以通过向分散了该复合钨氧化物的微粒(B成分)的溶液中添加上述金属的醇盐,覆盖复合钨氧化物微粒(B成分)的表面。
另外,优选复合钨氧化微粒(B成分)被分散剂覆盖。作为分散剂,可举出聚碳酸酯,聚砜、聚丙烯腈、聚芳酯、聚乙烯、聚氯乙烯、聚偏二氯乙烯、氟树脂、聚乙烯醇缩丁醛、聚乙烯醇、聚苯乙烯、有机硅系树脂、它们的衍生物等。通过用这些覆盖,向树脂添加时的分散性提高,进而具有防止机械物性的降低的效果。应予说明,作为分散剂的覆盖方法,可举出将复合钨氧化微粒(B成分)和分散剂溶解于甲苯等溶剂中,搅拌制备分散液后,用真空干燥等处理将溶剂除去,覆盖复合钨氧化微粒(B成分)的方法等。
另外,作为将B成分添加到聚碳酸酯树脂(A成分)的方法,可举出直接添加复合钨氧化物微粒(B成分)或经覆盖的复合钨氧化物微粒(B成分)的方法、用1~100倍的聚碳酸酯树脂(A成分)稀释后添加的方法。
B成分的含量相对于A成分100重量份为0.0001~0.2重量份,优选0.001~0.1重量份,更优选0.002~0.05重量份。B成分的含量少于0.0001重量份时,不能充分发挥红外线的屏蔽能力,多于0.2重量份时,耐湿热性恶化,另外,总透光率变得非常小。
(C成分:环氧树脂)
出于在保持高的透明性的同时、具有耐湿热性良好的红外线屏蔽性能的目的,本发明的树脂组合物含有环氧树脂作为C成分。使用的环氧树脂优选为含有缩水甘油基的环氧聚合物,更优选为共聚物含有甲基丙烯酸缩水甘油酯的环氧聚合物,共聚物的另一个成分优选使用聚苯乙烯。其中,优选使用聚甲基丙烯酸缩水甘油酯―聚苯乙烯共聚物。使用不含缩水甘油基的环氧聚合物时,有时与A成分的相容性变差,透明性差。作为含有缩水甘油基的聚合物的单体成分,可举出烯丙基缩水甘油醚、甲基丙烯酸缩水甘油酯、丙烯酸缩水甘油酯、4-羟基丁基丙烯酸酯缩水甘油醚、1,2-环氧―5-己烯、1,2-环氧―9-癸烯、环氧琥珀酸等,作为聚合物,可举出末端环氧改性聚二甲基硅氧烷、侧链环氧改性聚二甲基硅氧烷等。
C成分的含量相对于A成分100重量份为0.0001~0.1重量份,优选为0.001~0.05重量份,更优选为0.001~0.03重量份。如果含量低于0.0001重量份,则不体现充分的耐湿热性,超过0.1重量份时,色调恶化,损害透明性。
(D成分:脱模剂)
出于在保持高的透明性的同时具有耐湿热性良好的红外线屏蔽性能的目的,本发明的树脂组合物含有以由脂肪酸和多元醇构成的全酯为主成分的脂肪酸酯即脱模剂作为D成分。
上述脂肪酸的碳原子数优选为3~32,特别优选碳原子数为10~32的脂肪酸。作为该脂肪酸,可以举出例如癸酸、十一烷酸、十二烷酸、十三烷酸、十四烷酸、十五烷酸、十六烷酸(棕榈酸)、十七烷酸、十八烷酸(硬脂酸)、十九烷酸、山萮酸、二十烷酸、以及二十二烷酸等饱和脂肪族羧酸、以及棕榈油酸、油酸、亚油酸、亚麻酸、二十碳烯酸、二十碳五烯酸、以及鲸蜡烯酸等不饱和脂肪酸。其中,脂肪酸优选碳原子数为14~20。尤其优选饱和脂肪酸。特别优选硬脂酸和棕榈酸。硬脂酸、棕榈酸等上述的脂肪酸通常由牛油、猪油等所代表的动物性油脂和棕榈油、葵花籽油所代表的植物性油脂等天然油脂类制造,因此这些脂肪酸通常为含有碳原子数不同的其他羧酸成分的混合物。因此本发明的脂肪酸酯的制造中,优选使用由上述天然油脂类制造、且由含有其他的羧酸成分的混合物的形态构成的脂肪酸,特别是硬脂酸、棕榈酸。
作为上述多元醇,可举出季戊四醇、二季戊四醇、三季戊四醇、聚甘油(三甘油~六甘油)、双三羟甲基丙烷、木糖醇、山梨糖醇和甘露糖醇等。本发明的脂肪酸酯中,优选二季戊四醇。
本发明的脂肪酸酯为全酯。使用部分酯时,不体现充分的耐湿热性。从热稳定性方面考虑,本发明的脂肪酸酯的酸值优选为20以下,更优选为4~20的范围,进一步优选为4~12的范围。应予说明,酸值实质上可以为0。另外,脂肪酸酯的羟值优选0.1~30的范围。此外,碘值优选10以下。应予说明,碘值实质上可以为0。这些特性可以利用JIS K 0070规定的方法求出。
基于上述,D成分优选为下述式(1)表示的脂肪酸酯。
(式中,上述R1~R6各自独立地相同或不同,为碳原子数10~32的烷基。)
D成分的含量相对于A成分100重量份为0.001~0.5重量份,优选为0.01~0.4重量份,更优选为0.05~0.3重量份。如果含量低于0.001重量份,则不体现充分的耐湿热性,超过0.5重量份时,成型时聚碳酸酯树脂组合物的分子量降低。
(E成分:热稳定剂)
本发明的树脂组合物优选含有热稳定剂作为E成分。作为热稳定剂,优选选自酚系稳定剂(E-1成分)、硫系稳定剂(E-2成分)和磷系稳定剂(E-3成分)中的至少一种的热稳定剂。E成分的含量相对于A成分100重量份,优选为0.0002~0.8重量份,更优选为0.001~0.7重量份,进一步优选为0.01~0.1重量份。含量低于0.0002重量份时,有时不体现热稳定性的效果,如果超过0.8重量份,则与复合钨氧化物微粒并用时有时无法维持成型时的色调稳定性。
(E-1成分:酚系稳定剂)
作为酚系稳定剂,例如,可例示α-生育酚、丁基羟基甲苯、芥子醇、维生素E、正十八烷基-β-(4’-羟基-3’,5’-二-叔丁基苯基)丙酸酯、2-叔丁基-6-(3’-叔丁基-5’-甲基-2’-羟基苄基)-4-甲基苯基丙烯酸酯、2,6-二-叔丁基-4-(N,N-二甲基氨基甲基)苯酚、3,5-二-叔丁基-4-羟基苄基膦酸二乙酯、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’-亚甲基双(2,6-二-叔丁基苯酚)、2,2’-亚甲基双(4-甲基-6-环己基苯酚)、2,2’-二亚甲基-双(6-α-甲基-苄基-对甲酚)、2,2’-亚乙基-双(4,6-二-叔丁基苯酚)、2,2’-亚丁基-双(4-甲基-6-叔丁基苯酚)、4,4’-亚丁基双(3-甲基-6-叔丁基苯酚)、三甘醇-N-双-3-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯、1,6-己二醇双[3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯]、双[2-叔丁基-4-甲基6-(3-叔丁基-5-甲基-2-羟基苄基)苯基]对苯二甲酸酯、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、4,4’-硫代双(6-叔丁基-间甲酚)、4,4’-硫代双(3-甲基-6-叔丁基苯酚)、2,2’-硫代双(4-甲基-6-叔丁基苯酚)、双(3,5-二-叔丁基-4-羟基苄基)硫化物、4,4’-二-硫代双(2,6-二-叔丁基苯酚)、4,4’-三-硫代双(2,6-二-叔丁基苯酚)、2,2-硫代二亚乙基双-[3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯]、2,4-双(正辛硫基)-6-(4-羟基-3’,5’-二-叔丁基苯胺基)-1,3,5-三嗪、N,N’-六亚甲基双-(3,5-二-叔丁基-4-羟基氢化肉桂酰胺)、N,N’-双[3-(3,5-二-叔丁基-4-羟基苯基)丙酰基]肼、1,1,3-三(2-甲基-4-羟基-5-叔丁基苯基)丁烷、1,3,5-三甲基-2,4,6-三(3,5-二-叔丁基-4-羟基苄基)苯、三(3,5-二-叔丁基-4-羟基苯基)异氰脲酸酯、三(3,5-二-叔丁基-4-羟基苄基)异氰脲酸酯、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)异氰脲酸酯、1,3,5-三2[3(3,5-二-叔丁基-4-羟基苯基)丙酰氧基]乙基异氰脲酸酯以及四[亚甲基-3-(3’,5’-二-叔丁基-4-羟基苯基)丙酸酯]甲烷等。这些均容易得到。上述酚系稳定剂可以单独或者组合2种以上使用。
(E-2成分:硫系稳定剂)
作为硫系化合物,可举出二月桂基硫代二丙酸酯、双十三烷基硫代二丙酸酯、二肉豆蔻基硫代二丙酸酯、二硬脂基硫代二丙酸酯、季戊四醇四(3-月桂基硫代丙酸酯)、季戊四醇四(3-十二烷基硫代丙酸酯)、季戊四醇四(3-十八烷基硫代丙酸酯)、季戊四醇四(3-肉豆蔻基硫代丙酸酯)、季戊四醇四(3-十八烷基硫代丙酸酯)等。这些可以单独使用,也可以混合2种以上使用。
(E-3成分:磷系稳定剂)
磷系稳定剂作为芳香族聚碳酸酯的热稳定剂已经广为人知。本发明中,磷系稳定剂可以提高其热稳定性直到树脂组合物能耐受极其苛刻的热负荷的程度。作为磷系稳定剂,主要举出亚磷酸酯化合物和亚膦酸酯。
这里,作为亚磷酸酯化合物,例如,可例示亚磷酸三苯酯、亚磷酸三(壬基苯基)酯、亚磷酸三癸酯、亚磷酸三辛基酯、亚磷酸三(十八烷基)酯、二癸基单苯基亚磷酸酯、二辛基单苯基亚磷酸酯、二异丙基单苯基亚磷酸酯、单丁基二苯基亚磷酸酯、单癸基二苯基亚磷酸酯、单辛基二苯基亚磷酸酯、2,2-亚甲基双(4,6-二-叔丁基苯基)辛基亚磷酸酯、三(二乙基苯基)亚磷酸酯、三(二-异丙基苯基)亚磷酸酯、三(二-n-丁基苯基)亚磷酸酯、三(2,4-二-叔丁基苯基)亚磷酸酯、三(2,6-二-叔丁基苯基)亚磷酸酯、二硬脂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(2,6-二-叔丁基-4-乙基苯基)季戊四醇二亚磷酸酯、苯基双酚A季戊四醇二亚磷酸酯、双(壬基苯基)季戊四醇二亚磷酸酯、二环己基季戊四醇二亚磷酸酯等。
此外,作为其他亚磷酸酯化合物,也可以使用与二元酚类反应具有环状结构的亚磷酸酯化合物。例如,可例示2,2’-亚甲基双(4,6-二-叔丁基苯基)(2,4-二-叔丁基苯基)亚磷酸酯、2,2’-亚甲基双(4,6-二-叔丁基苯基)(2-叔丁基-4-甲基苯基)亚磷酸酯、2,2’-亚甲基双(4-甲基-6-叔丁基苯基)(2-叔丁基-4-甲基苯基)亚磷酸酯、2,2’-亚乙基双(4-甲基-6-叔丁基苯基)(2-叔丁基-4-甲基苯基)亚磷酸酯等。
作为亚膦酸酯化合物,例如可举出四(2,4-二-叔丁基苯基)-4,4’-亚联苯基二亚膦酸酯、四(2,4-二-叔丁基苯基)-4,3’-亚联苯基二亚膦酸酯、四(2,4-二-叔丁基苯基)-3,3’-亚联苯基二亚膦酸酯、四(2,6-二-叔丁基苯基)-4,4’-亚联苯基二亚膦酸酯、四(2,6-二-叔丁基苯基)-4,3’-亚联苯基二亚膦酸酯、四(2,6-二-叔丁基苯基)-3,3’-亚联苯基二亚膦酸酯、双(2,4-二-叔丁基苯基)-4-苯基-苯基亚膦酸酯、双(2,4-二-叔丁基苯基)-3-苯基-苯基亚膦酸酯、双(2,6-二-正丁基苯基)-3-苯基-苯基亚膦酸酯、双(2,6-二-叔丁基苯基)-4-苯基-苯基亚膦酸酯、双(2,6-二-叔丁基苯基)-3-苯基-苯基亚膦酸酯等,优选四(二-叔丁基苯基)-亚联苯基二亚膦酸酯、双(二-叔丁基苯基)-苯基-苯基亚膦酸酯,更优选四(2,4-二-叔丁基苯基)-亚联苯基二亚膦酸酯、双(2,4-二-叔丁基苯基)-苯基-苯基亚膦酸酯。上述亚膦酸酯化合物能够与2个以上烷基被取代的具有芳基的亚磷酸酯化合物并用,因而优选。
(F成分:紫外线吸收剂)
本发明的树脂组合物有时不实施涂装等就可以使用。上述情况下,有时要求良好的耐光性,因此优选配合紫外线吸收剂。
作为紫外线吸收剂,优选选自苯并三唑系紫外线吸收剂(F-1成分)、三嗪系紫外线吸收剂(F-2成分)以及嗪系紫外线吸收剂(F-3成分)中的至少一种的紫外线吸收剂。F成分的含量相对于A成分100重量份,优选为0.1~2重量份,更优选为0.12~1.5重量份,进一步优选为0.15~1重量份。如果F成分的含量小于0.1重量份,则有时不体现充分的耐光性,多于2重量份时,有时产生由气体产生所致的外观不良、物性降低。
(F-1成分:苯并三唑系紫外线吸收剂)
作为苯并三唑系紫外线吸收剂,例如,可例示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-3,5-二枯基苯基)苯基苯并三唑、2-(2-羟基-3-叔丁基-5-甲基苯基)-5-氯苯并三唑、2,2’-亚甲基双[4-(1,1,3,3-四甲基丁基)-6-(2H-苯并三唑-2-基)苯酚]、2-(2-羟基-3,5-二-叔丁基苯基)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-3,5-二-叔戊基苯基)苯并三唑、2-(2-羟基-5-叔辛基苯基)苯并三唑、2-(2-羟基-5-叔丁基苯基)苯并三唑、2-(2-羟基-4-辛氧基苯基)苯并三唑、2,2’-亚甲基双(4-枯基-6-苯并三唑苯基)、2,2’-对亚苯基双(1,3-苯并嗪-4-酮)和2-[2-羟基-3-(3,4,5,6-四氢邻苯二甲酰亚胺甲基)-5-甲基苯基]苯并三唑、以及2-(2’-羟基-5-甲基丙烯酰氧基乙基苯基)-2H-苯并三唑与可与该单体共聚的乙烯基系单体的共聚物、2-(2’―羟基-5-丙烯酰氧基乙基苯基)―2H―苯并三唑与可与该单体共聚的乙烯基系单体的共聚物等,具有2-羟基苯基-2H-苯并三唑骨架的聚合物等。
(F-2成分:三嗪系紫外线吸收剂)
作为三嗪系紫外线吸收剂,例如,可例示2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-己氧基苯酚、2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-甲基氧基苯酚、2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-乙基氧基苯酚、2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-丙基氧基苯酚以及2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-丁基氧基苯酚等。进而可例示2-(4,6-双(2,4-二甲基苯基)-1,3,5-三嗪-2-基)-5-己氧基苯酚等、上述例示化合物的苯基为2,4-二甲基苯基的化合物。
(F-3成分:嗪系紫外线吸收剂)
作为嗪系紫外线吸收剂,例如,可例示2,2’-对亚苯基双(3,1-苯并/>嗪-4-酮)、2,2’-间亚苯基双(3,1-苯并/>嗪-4-酮)、2,2’-p,p’-二亚苯基双(3,1-苯并/>嗪-4-酮)等。
(其他成分)
(1)染颜料
本发明的树脂组合物能够提供含有各种染颜料而体现多样的设计性的成型品。作为本发明中使用的染颜料,可以举出苝系染料、香豆素系染料、硫靛系染料、蒽醌系染料、噻吨酮系染料、普鲁士蓝等亚铁氰化物、芘酮系染料、喹啉系染料、喹吖啶酮系染料、二嗪系染料、异吲哚啉酮系染料、酞菁系染料、炭黑、氧化钛、氧化锌、硫化锌、碳酸钙、金属氧化物微粒等。此外,本发明的聚碳酸酯树脂组合物也能够配合金属颜料,而得到更良好的金属色彩。作为金属颜料,优选铝粉。另外,通过配合荧光增白剂、或除此之外的可发光的荧光染料,能够赋予发出发光色的更良好的设计效果。作为本发明中使用的荧光染料(包含荧光增白剂),例如,可以举出香豆素系荧光染料、苯并吡喃系荧光染料、苝系荧光染料、蒽醌系荧光染料、硫靛系荧光染料、呫吨系荧光染料、呫吨酮系荧光染料、噻吨系荧光染料、噻吨酮系荧光染料、噻嗪系荧光染料以及二氨基茋系荧光染料等。其中,优选耐热性良好且聚碳酸酯树脂的成型加工时的劣化少的香豆素系荧光染料、苯并吡喃系荧光染料以及苝系荧光染料。
(2)氮化物微粒
本发明的树脂组合物优选含有氮化物微粒。氮化物微粒优选为选自Ti、Zr、Hf、V、Nb以及Ta中的至少一种的金属的氮化物微粒。
(树脂组合物的制造)
制造本发明的树脂组合物时,可采用任意的方法。例如可以举出将各成分以及任意其他成分预备混合,其后熔融混炼,进行颗粒化的方法。作为预备混合的手段,可以举出Nauter搅拌机、V型搅拌机、亨舍尔搅拌机、机械化学装置、挤出混合机等。预备混合也可以根据情况利用挤出造粒器、压块机等进行造粒。预备混合后,利用排气式双轴挤出机为代表的熔融混炼机进行熔融混炼,以及造粒机等机器进行颗粒化。作为熔融混炼机,还可以举出班伯里密炼机、混炼辊、恒热搅拌容器等,优选排气式双轴挤出机。此外,也可以采取不将各成分和任意的其他成分进行预备混合而各自独立地供给双轴挤出机所代表的熔融混炼机的方法。
(成型品的制造)
如上得到的本发明的树脂组合物通常可以将如上制造的颗粒进行注塑成型而制造各种制品。此外也可以不经由颗粒而将用挤出机熔融混炼的树脂直接制成片材、膜、特殊形状挤出成型品以及注塑成型品。
上述注塑成型中,不仅有通常的成型方法,还可以适当地根据目的使用注射压缩成型、注射加压成型、气体辅助注塑成型、发泡成型(包括基于超临界流体的注入的发泡成型)、嵌件成型、模内涂层成型、隔热模具成型、迅速加热冷却模具成型、双色成型、夹层成型,以及超高速注塑成型等注塑成型法得到成型品。这些各种成型法的优点已经广为人知。另外,成型也可以选择冷流道方式和热流道方式中任一种。另外,本发明的树脂组合物也可以利用挤出成型而成型为各种特殊形状挤出成型品、片材。另外,优选对成型品的单面或者两面实施硬涂处理。
成型品的厚度优选为0.1~20mm,更优选为0.1~15mm。另外,成型品的ISO9050规定的总透光率优选为20%以上,更优选为30%以上。并且,成型品的ISO9050规定的雾度优选为5%以下,更优选为3%以下。
本发明人实施的形态是将上述的各要件的优选范围集合而得的形态,例如,在下述的实施例中记载其代表例。当然,本发明不限于这些形态。
实施例
以下,举出实施例对本发明进一步进行具体说明。另外,以下只要没有特别说明,“份”就表示“重量份”,%就表示“重量%”。
(1)树脂组合物的制作
(1-1)使用原料
(A成分)
A-1:由下述制法得到的分子量24200的聚碳酸酯树脂粉末
在带挡板的反应容器中,安装三级六叶的搅拌机和回流冷却管。在该反应容器中加入双酚A45.6份、相对于双酚A为2.78摩尔%的对叔丁基苯酚,二氯甲烷265份和水200份,进行氮气吹扫而将反应容器内的氧除去。应予说明,上述阶段中反应容器中的内容物小于容器容量的80%。接下来,向上述悬浮液供给约80份用于供给连二亚硫酸钠0.09份和氢氧化钠21.8份的水溶液,在15℃溶解双酚A。搅拌下,用30分钟向该混合物供给光气23.35份。其后,添加三乙胺0.016份(相对于双酚A为0.08摩尔%)搅拌60分钟,结束反应。其后,静置反应混合物,对有机相进行分液。向得到的聚碳酸酯树脂的二氯甲烷溶液加入二氯甲烷制成14重量%的浓度的溶液,再使用带多孔板离心萃取机(川崎工程株式会社制KCC离心萃取机)以流量1000ml/min的速度供给0.5%氢氧化钠水溶液,以流量1000ml/min的速度供给有机相,在3500rpm的条件下处理后,使有机相为盐酸酸性,其后反复水洗,水相的电导率达到与离子交换水几乎相同时,将二氯甲烷蒸发,得到聚碳酸酯树脂粉末。
(B成分)
B-1:由Cs0.33WO3约23重量%和有机分散树脂构成的热线吸收剂(住友金属矿山株式会社制YMDS-874R)
(C成分)
C-1:环氧树脂(日油株式会社制:G-0250SP)
C-2:环氧树脂(日油株式会社制:G-0150M)
(D成分)
D-1:脂肪酸全酯(具有式(1)表示的结构。)(理研维他命株式会社制:L-8483)
D-2:脂肪酸全酯(具有式(1)表示的结构。)(理研维他命株式会社制:SL-02)
D-3:脂肪酸全酯(不具有式(1)表示的结构。)(日油株式会社制:H-874S)
D-4:脂肪酸部分酯(理研维他命株式会社制:S-100A)
(E成分)
E-1:酚系稳定剂(BASF Japan株式会社制:IRGANOX 1076)
E-2:硫系稳定剂:(BASF Japan株式会社制:IRGANOX L115)
E-3:磷系稳定剂(Clariant Japan株式会社制:P-EPQ)
(F成分)
F-1:苯并三唑系紫外线吸收剂(ChemiPro Kasei株式会社制:Chemisorb 79)
F-2:苯并三嗪系紫外线吸收剂(BASF Japan株式会社制:Tinuvin 1577ED)
F-3:嗪系紫外线吸收剂(锦海化学株式会社制:UV0901)/>
(2)试验片制作
(2-1)树脂组合物的制造
按表1和表2记载的比例计量表1和表2记载的各成分,用混合搅拌机混合后,使用排气式双轴挤出机熔融混炼,得到聚碳酸酯树脂组合物的颗粒。应予说明,B成分的含量为括号内示出的B-1中含有的无机系紫外线吸收材料Cs0.33WO3的量。(括号外的数字表示B-1的树脂组合物中的重量份。)聚碳酸酯树脂中添加的添加剂分别预先以配合量的10~100倍的浓度制作成与聚碳酸酯树脂的预备混合物后,用搅拌机进行全体的混合。排气式双轴挤出机使用株式会社日本制钢所制:TEX30α(完全啮合,同向旋转,2根螺杆)。混炼区域为排气口近前1个位置的类型。挤出条件为排出量20kg/h,螺杆转速130rpm,排气口真空度3kPa,另外,挤出温度从第1供给口到模头部分为290℃。应予说明,上述的树脂组合物的制造在通过HEPA过滤器的洁净的空气循环的气氛中实施,另外,作业时充分注意不混入异物。
(2-2)试验片制作方法
将得到的颗粒在110~120℃用6小时热风循环式干燥机进行干燥后,利用注塑成型机[住友重机械工业株式会社制SG260M-HP],在料筒温度300℃、模具温度80℃的条件下成型出作为评价用的试验片的宽度150mm×长度150mm×厚度5mm的板。
(3)评价项目
(3-1)试验片的粘均分子量
将粉碎为3mm见方左右的刨花的试验片和其20~30倍重量的二氯甲烷混合,使组合物中的可溶成分溶解。接下来,通过硅藻土过滤收集上述可溶成分。然后,除去得到的溶液中的溶剂,将除去溶剂后的固体充分干燥,得到溶解于二氯甲烷的成分的固体。由将上述固体0.7g溶解在二氯甲烷100ml而得的溶液,与上述的聚碳酸酯树脂的粘均分子量同样地求出20℃的比粘度,由该比粘度计算粘均分子量。
(3-2)耐湿热性试验后的红外线屏蔽性能的变化量
从试验片切出50mm见方的试验片。对其光谱射线使用株式会社Hitachi High-Technologies Corporation制分光光线测量仪U-4100,根据ISO13837计算初始的Totaltransmission of solar energy(Tts)。将结果示于表1和表2。接下来,用压力锅试验机TPC-412(ESPEC株式会社制)在120℃、75%Rh的条件下对上述试验片进行48小时的湿热处理,用与上述方法相同的方法计算Tts。计算压力锅后的Tts与初始的Tts之差,作为耐湿热性试验后的红外线屏蔽性能的变化量(ΔTts)。将结果示于表1和表2。
(3-3)总透光率和雾度
从试验片切出50mm见方的试验片,使用株式会社村上色彩技术研究所制雾度计HR-100根据ISO13468测定总透光率和雾度。将结果示于表1和表2。
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Claims (11)
1.一种树脂组合物,相对于(A)聚碳酸酯树脂即A成分100重量份,含有(B)通式MxWyOz表示的复合钨氧化物微粒即B成分0.02~0.15重量份、(C)含有缩水甘油基的环氧聚合物即C成分0.001~0.08重量份以及(D)作为以由脂肪酸和多元醇构成的全酯为主成分的脂肪酸酯的脱模剂即D成分0.1~0.4重量份,在通式MxWyOz中,M为选自碱金属中的1种以上的元素,W为钨,O为氧,0.001≤x/y≤1,2.2≤z/y≤3.0;
所述D成分为由下述式(1)表示的脂肪酸酯,
式中,所述R1~R6各自独立地相同或不同,且为碳原子数10~32的烷基。
2.根据权利要求1所述的树脂组合物,其特征在于,B成分的粒径为1nm~800nm。
3.根据权利要求1或2所述的树脂组合物,其特征在于,相对于A成分100重量份,含有(E)热稳定剂即E成分0.0002~0.8重量份。
4.根据权利要求3所述的树脂组合物,其特征在于,E成分为选自酚系稳定剂即E-1成分、硫系稳定剂即E-2成分以及磷系稳定剂即E-3成分中的至少一种的热稳定剂。
5.根据权利要求1或2所述的树脂组合物,其特征在于,相对于A成分100重量份,含有(F)紫外线吸收剂即F成分0.1~2重量份。
6.根据权利要求5所述的树脂组合物,其特征在于,F成分为选自苯并三唑系紫外线吸收剂即F-1成分、三嗪系紫外线吸收剂即F-2成分和嗪系紫外线吸收剂即F-3成分中的至少一种的紫外线吸收剂。
7.一种膜、片材或注塑成型品,由权利要求1~6中任一项所述的树脂组合物构成。
8.根据权利要求7所述的成型品,厚度为0.1~20mm。
9.根据权利要求7或8所述的成型品,其中,由ISO9050规定的总透光率为20%以上,由ISO9050规定的雾度为5%以下。
10.一种成型品,是对权利要求7或8所述的成型品的单面或者两面实施硬涂处理而得的。
11.根据权利要求7或8所述的成型品,其中,成型品为车辆用灯具、车辆用传感器罩、车辆用显示装置罩、车辆用窗构件、继电器用显示装置罩或者建筑材料用窗构件。
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