CN106945375A - 一种吸声阻尼泡沫夹芯复合材料及其制造方法 - Google Patents
一种吸声阻尼泡沫夹芯复合材料及其制造方法 Download PDFInfo
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Abstract
本发明公开了一种吸声阻尼泡沫夹芯复合材料及其制造方法,由芯材、面材和阻尼涂层构成。芯材为一种开孔聚氨酯‑聚酰亚胺泡沫板,面材为阻燃玻璃纤维布外护水性聚氨酯内舱涂料,阻尼层为聚醚型聚氨酯弹性体。在频率250~6000Hz,板厚25mm时的平均吸声系数为0.42~0.46,极限氧指数≥32,烟密度 Dm≤50,自由阻尼损耗因子大于1.0,粘接强度N/25mm,泡沫材料层破坏。
Description
技术领域
本发明涉及一种泡沫夹芯复合材料,属于聚合物基轻质复合材料范畴,具体涉及一种具有复合结构的聚氨酯-聚酰亚胺泡沫夹芯吸声阻尼材料及其制造方法。
背景技术
泡沫夹芯材料在二十世纪四十年代就已作为复合材料使用,聚氨酯泡沫夹芯板,它具有质量轻、比强度高、良好的抗冲击吸能特性,已广泛用于建材行业。玻璃棉夹芯板具有良好的吸声、隔声、耐温、阻燃特性,广泛用于建筑、船舶、海洋工程平台的隔声吸声场合。聚氨酯-聚酰亚胺泡沫材料具有良好的吸声、隔声性能,耐温、阻燃、低烟密度是一种可替代超细玻璃棉且对人体无害的泡沫吸声材料,合理地在材料表面涂膜可以提高其低频段的吸声性能。泡沫夹芯吸声阻尼复合材料能够削弱噪音与震动,具有隔音、绝热、减振、降噪、抗疲劳等性能。目前在航空、航天、航海及海洋工程领域对具有低密度、吸声阻尼减振降噪复合材料的需求不断增加,由于夹芯复合材料具有良好的比强度、大阻尼特性,广泛应用于舰艇、潜水器、海洋工程平台的吸声、阻尼、减振、降噪等领域。
中国专利CN 201110037996.X报导了一种夹心阻尼复合材料,由外层、内层和阻尼层构成。其中外层为结构层,是一种高刚度纤维增强树脂基复合材料,内层为夹心层,由硬质泡沫塑料构成。阻尼层位于结构层与结构层之间或位于结构层与夹心层之间。材料的外层和内层共同构成夹心结构,以提供材料整体的刚度和强度,使材料具有较高的结构阻尼减振降噪性能。
中国专利CN200810054400.5涉及一种泡沫夹芯整体结构复合材料及其制备方法。该复合材料包括上面层、下面层和泡沫夹芯层,泡沫夹芯层与上、下面层用缝合线缝合为一个整体,并采用树脂传递模塑工艺一次注射成型,上面层和下面层的外表面平整光滑。本发明的复合材料整体性好,使用寿命长,形状结构尺寸精确,并且力学性能优良。
中国专利CN201510024686.2一种环氧泡沫夹芯复合材及其制造方法。该夹芯复合材料由芯材、面材和阻尼层构成。芯材为一种空心玻璃微珠增强环氧泡沫塑料,面材为玻纤网格布增强环氧玻璃钢,阻尼层为聚醚型聚氨酯弹性体。本发明的夹芯复合材料采用具有优良粘结性能和阻尼性能的聚氨酯弹性体,作为泡沫芯材与芯材、芯材与面材之间的黏结阻尼层,制得的泡沫夹芯结构复合材料,具有质量轻、强度高、绝热、阻尼、减振、降噪一体化功能,从而提升材料的综合性能。
以上专利均未涉及到具有耐温、阻燃、低烟、低毒、吸声、阻尼、减振、降噪功能一体化的聚氨酯-聚酰亚胺泡沫夹心复合材料的制备方法。
发明内容
本发明所要解决的技术问题是:提供一种低密度、低烟密度、耐温、阻燃、吸声、阻尼、减振、降噪夹心复合结构材料。
为解决上述技术问题,本发明采用的技术方案是:
本发明提供的吸声阻尼泡沫夹芯复合材料,包括外层、内层和阻尼层,其中材料的外层为结构层,由纤维布增强聚氨酯弹性体构成;材料的内层为夹芯层,由开孔聚氨酯-聚酰亚胺泡沫组成;阻尼层位于外层与内层之间;
制备方法如下:聚氨酯-聚酰亚胺泡沫体作为芯材,表面涂布阻尼涂层,涂层外表面敷贴面材经室温或加温固化,制备具有吸声阻尼复合结构的泡沫夹芯材料。
所述的开孔聚氨酯-聚酰亚胺泡沫由下列重量份数的组分制成:
制备工艺为:
在备有搅拌器、温度计及回流冷凝器的三口瓶中,投入芳香二酐和极性溶剂,充分搅拌并缓慢升温,待固体芳香二酐全部溶解,加入胺化物反应至清澈溶液时,降温加入脂肪醇进行回流酯化反应,制得清澈透明二酸二酯溶液。降温到60℃以下,加入催化剂将溶液搅拌到恒温,制得前驱体溶液。
前驱体溶液按比例加入聚醚多元醇、泡沫稳定剂、催化剂、发泡剂、阻燃剂配制泡沫组合溶液。泡沫组合溶液与异氰酸酯指数是1.0~1.05的多异氰酸酯快速搅拌均匀。倒入模具中自由发泡反应制得泡沫中间体,泡沫中间体脱粘后脱模,从模具中取出,放入微波炉或电热鼓风干燥箱中固化,制得聚酰亚胺泡沫体,并测试泡沫性能。泡沫组合溶液与多异氰酸酯的重量比是100:100~105。
上述所述的芳香二酐包括:3,3,,4,4,-二苯醚四羧酸二酐(ODPA)、3,3,,4,4,-二苯甲酮四羧酸二酐(BTDA)、3,3,,4,4,-联苯四羧酸二酐(BPDA)、1,2,4,5-均苯四羧酸二酐(PMDA)。
胺化物包括:4,4,-二氨基二苯醚、3,3,-二氨基二苯基砜、4,4,-二氨基二苯基甲烷、2,6-二氨基吡啶、对苯二胺、端氨基聚醚(D-2000、T-403)。
聚醚多元醇包括:聚氧化丙烯多元醇牌号3050,羟值54.5~57.5mgkoH/g,水分≤0.05%,黏度/25℃≤700mpa.s;牌号330N,羟值33.5~36.5mgkoH/g,水分≤0.05%,黏度/25℃750~950mpa.s;蔗糖聚氧化丙烯多元醇牌号8010,羟值430~450mgkoH/g,水分≤0.1%,黏度/25℃4~7pa.s;牌号8305,羟值430~450mgkoH/g,水分≤0.1%,黏度/25℃6~9pa.s。
脂肪醇包括:甲醇、乙醇、低分子聚乙二醇。
极性溶剂包括:二甲基甲酰胺、二甲基乙酰胺、N-甲基吡咯烷酮。
泡沫稳定剂包括:非水解型水溶性聚醚硅氧烷(DC-193、DC-195、AK-8805、AK-8808)、聚氧化乙烯非离子表面活性剂、阳离子含氟表面活性剂、聚氧乙烯基醚氟碳泡沫稳定剂。
发泡剂包括:水、甲醇、乙二醇乙醚、乙二醇丁醚。
催化剂包括:三乙醇胺、三乙烯二胺、双(2-二甲氨基乙基)醚、辛酸亚锡、二月桂酸二丁基锡、异喹啉。
阻燃剂包括:三(2-氯乙基)磷酸酯、三(2-氯丙基)磷酸酯、甲级膦酸二甲酯、可膨胀石墨、三氧化二锑、聚磷酸铵、三聚氰胺磷酸酯、磷溴抑烟阻燃剂(FR-808)。
多异氰酸酯包括:多苯基多亚甲基多异氰酸酯(PAPI)、二苯基甲烷二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI-80/20)。
本发明中所述的阻尼层是一种聚醚型聚氨酯弹性体,由A、B两组份构成,A组份为异氰酸酯预聚体;B组份由聚醚多元醇、胺扩链剂、硅烷偶联剂、受阻酚功能助剂、阻尼填料、触变剂组成:
A组份异氰酸酯预聚体由聚醚多元醇和多异氰酸酯制备,两者的重量份数比是400:300。
制备方法如下:称取聚醚多元醇于1000ml三口瓶中,加热到100~110℃真空脱水1小时;降温到60~70℃,投入计量的多异氰酸酯,加热到80℃预聚反应2小时,出料置于密封容器中备用。
B组份的重量比:
聚醚多元醇 100份。
胺扩链剂 30份。
硅烷偶联剂 12份。
受阻酚功能助剂 35份。
阻尼填料 245份。
触变剂 1.5份。
制备方法如下:称量上述组分,于搅拌研磨分散机中研磨分散均匀制备B组份;
以A、B两组份按质量比1:2配制阻尼涂层。
阻尼层A组份中用的聚醚多元醇也选自上述的聚醚多元醇中。
胺扩链剂选自下列中的一种或多种的混合:二乙基甲苯二胺(E-100)、二甲硫基甲苯二胺(E-300)、2,4-二氨基-3,5-二甲硫基氯苯(TX-2)、双仲丁氨基二苯基甲烷(Unilink4200),N,N,-二烷基苯二胺(Unilink 4100)。
硅烷偶联剂选自下列中的一种或多种的混合:γ-氨丙基三甲氧基硅烷(KH--540)、γ-氨丙基三乙氧基硅烷(KH--550)、γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷(KH-560)、γ-(甲基丙烯酰氧基)丙基三甲氧基硅烷(KH—570)、γ-巰丙基三甲氧基硅烷(KH—580)、γ-巰丙基三乙氧基硅烷(KH—590)。
阻尼填料选自下列中的一种或多种的混合:云母粉(60~800目)、石墨粉(50~500目)、碳酸钙、硫酸钡、滑石粉、珍珠粉、氢氧化铝。
受阻酚功能助剂选自下列中的一种或2种的混合:四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(AO-60);3,9-双{1,1-二甲基-2[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基]乙基}-2,4,6,8-四氧杂螺环-(5,5)十一烷(AO-80)有机小分子杂化体。
触变剂是有机膨润土。
本发明的主要原理是利用芳香二酐的二酸二酯、胺化物及水与多异氰酸酯快速反应,其中水与多异氰酸酯反应生成中间产物,中间产物受热分解产生二氧化碳和胺化物。二氧化碳作为发泡剂,胺化物与芳香二酐的二酸二酯反应形成聚酰亚胺结构。配方中加入泡沫稳定剂用以稳定泡沫,加入泡沫催化剂加速发泡反应。异喹啉不仅催化发泡反应,而且提高酰亚胺的转化率,胺化物可直接与二酐的二酸二酯及多异氰酸酯反应,将醚的柔性链段引入到聚酰亚胺分子链上,提高了分子链的柔韧性,从而制得刚柔兼得的聚氨酯-聚酰亚胺泡沫体。
本发明的有益效果:
本发明由于采用阻尼聚氨酯弹性体黏接聚氨酯-聚酰亚胺泡沫体构成泡沫夹芯吸声阻尼芯材,面材为阻燃玻璃纤维布外护水性聚氨酯内舱涂料,制造的低密度、低烟密度、耐温、阻燃、吸声、阻尼夹芯复合材料实用效果好,应用范围更为广泛已达到本发明的目的。
本发明提供的低密度、低烟密度、耐温、阻燃、吸声、阻尼、减振、降噪夹心复合结构材料,其特点是采用开孔聚氨酯-聚酰亚胺泡沫材料,涂敷具有优良粘结性能和阻尼性能的聚氨酯弹性体阻尼涂层构成泡沫夹芯吸声、阻尼层,面材为阻燃玻璃纤维布外护水性聚氨酯内舱涂料,制得泡沫夹芯复合材料,比传统的聚氨酯泡沫夹芯板和玻璃棉夹芯板具有更高的耐温、阻燃、吸声、阻尼性能,使其应用范围更为广泛。材料的外层和内层共同构成夹芯结构以提供材料整体的刚度和强度,并具有一定的降低振动的作用,此外,夹芯层的存在还具有减重、吸声、隔音、阻尼、降噪的功能,该材料耐温、阻燃、低烟、低毒可以适应不同的功能需求。阻尼层的存在大大提高了材料的结构阻尼,使材料具有高阻尼的性质。
具体实施方式
实施例1
本实施例提供一种开孔聚氨酯-聚酰亚胺泡沫的制备:
在备有搅拌器、温度计及回流冷凝器的1000ml三口瓶中,投入170克1,2,4,5均苯四羧酸二酐(PMDA)及240克二甲基甲酰胺,充分搅拌缓慢升温到90~100℃,待1,2,4,5均苯四羧酸二酐固体颗粒全部溶解时,加入25克4,4,,二氨基二苯醚升温到120℃反应到清澈溶液。降温到65℃投入25克无水甲醇,进行酯化反应至红棕色透明溶液,降温到60℃以下,加入2.5克异喹啉,搅拌均匀,制得前驱体溶液。
称取100克上述前驱体溶液加入12克发泡剂去离子水,1.5克三乙烯二胺、0.5克双(二甲氨基乙基)醚催化剂,30克聚醚多元醇8010,2.5克聚氧乙烯基醚氟碳泡沫稳定剂,20克甲级膦酸二甲酯、15克三聚氰胺磷酸酯阻燃剂,配制成泡沫组合溶液。
泡沫组合溶液与异氰酸酯指数为1.0~1.05的多苯基多亚甲基多异氰酸酯快速搅拌均匀,倒入模具中自由发泡,泡沫体脱粘后脱模,放入电热鼓风干燥箱中,240℃固化1小时,制得聚氨酯-聚酰亚胺泡沫体。
泡沫组合溶液与多苯基多亚甲基多异氰酸酯的重量比是1:1。
测试泡沫的性能如下:
实施例2
本实施例提供一种开孔聚氨酯-聚酰亚胺泡沫的制备:
在备有搅拌器、温度计及回流冷凝器的1000ml三口瓶中,投入150克3,3,,4,4,,二苯甲酮四甲酸二酐(BTDA)及210克二甲基甲酰胺,充分搅拌缓慢升温到100~110℃,待3,3,,,4,4,,二苯甲酮四甲酸二酐(BTDA)固体颗粒全部溶解,加入25克4,4,,二氨基二苯醚(4,4,,-ODA)升温到120℃反应到清澈溶液溶液,降温到65℃投入38克无水甲醇,进行酯化反应,待溶液清澈透明,降温到60℃以下。加入2.5克异喹啉,将溶液搅拌均匀,制得淡黄色透明前驱体溶液。
称取100克上述前驱体溶液加入12克去离子水,1.5克三乙烯二胺、0.5克双(二甲氨基乙基)醚催化剂,30克聚醚多元醇8305,1.5克聚氧乙烯基醚氟碳泡沫稳定剂及2.0非水解型水溶性聚醚硅氧烷DC-193泡沫稳定剂,20克甲级膦酸二甲酯、15克三氧化二锑阻燃剂,配制成泡沫组合溶液。泡沫组合溶液与异氰酸酯指数为1.0~1.05的多苯基多亚甲基多异氰酸酯快速搅拌均匀,倒入模具中自由发泡,泡沫体脱粘后脱模,放入电热鼓风干燥箱中,240℃固化1小时,制得聚氨酯-聚酰亚胺泡沫体。
泡沫组合溶液与多苯基多亚甲基多异氰酸酯的重量比是100:105。
测试泡沫的性能如下:
实施例3
本实施例提供一种开孔聚氨酯-聚酰亚胺泡沫的制备:
在备有搅拌器、温度计及回流冷凝器的1000ml三口瓶中,投入170克1,2,4,5均苯四羧酸二酐(PMDA)及260克二甲基甲酰胺,充分搅拌缓慢升温到90~100℃,待1,2,4,5均苯四羧酸二酐固体颗粒全部溶解,溶液变得澄清时,降温到65℃投入25克无水甲醇,进行酯化反应,待溶液清澈透明,降温到60℃以下。加入2.5克异喹啉,30克聚氧化丙烯二胺(D-2000)。将上述溶液搅拌至恒温,制得棕红色透明粘稠前驱体溶液。
称取100克上述前驱体溶液加入12克发泡剂去离子水,1.5克三乙烯二胺、0.5克双(二甲氨基乙基)醚催化剂,30克聚醚多元醇3050,2.5克聚氧乙烯基醚氟碳泡沫稳定剂,20克甲级膦酸二甲酯、15磷溴抑烟阻燃剂(FR-808)克阻燃剂,配制成泡沫组合溶液。泡沫组合溶液与异氰酸酯指数为1.0~1.05的多苯基多亚甲基多异氰酸酯快速搅拌均匀,倒入模具中自由发泡,泡沫体脱粘后脱模,放入电热鼓风干燥箱中,240℃固化1小时,制得聚氨酯-聚酰亚胺泡沫板。
泡沫组合溶液与多苯基多亚甲基多异氰酸酯的重量比是100:103。
测试泡沫的性能如下:
实施例4
本实施例提供一种开孔聚氨酯-聚酰亚胺泡沫的制备:
在备有搅拌器、温度计及回流冷凝器的1000ml三口瓶中,投入180克3,,3,,4,,4,联苯四羧酸二酐(BPDA)及260克二甲基甲酰胺,充分搅拌缓慢升温到100~110℃,加入22克2.6二氨基吡啶(DAP),继续升温到130℃,使3,3,,,4,4,,联苯四羧酸二酐及4,4,,二氨基吡啶固体颗粒全部溶解,溶液变得澄清时,降温到65℃投入34克无水甲醇,进行酯化反应,待溶液清澈透明,降温到60℃以下。加入2.5克异喹啉,25克聚氧化丙烯三胺(T-403)。将上述溶液搅拌至恒温,制得枣红色透明粘稠前驱体溶液。
称取100克上述前驱体溶液加入12克发泡剂去离子水,1.0克三乙烯二胺、0.5克双(二甲氨基乙基)醚、0.5克二月桂酸二丁基锡催化剂,30克聚醚多元醇330N,1.5克聚氧乙烯基醚氟碳泡沫稳定剂及2.5克非水解型水溶性聚醚硅氧烷AK-8805泡沫稳定剂,10克甲级膦酸二甲酯、15克磷溴抑烟阻燃剂(FR-808)、10克三聚氰胺磷酸酯阻燃剂,配制成泡沫组合溶液。泡沫组合溶液与异氰酸酯指数为1.0~1.05的多苯基多亚甲基多异氰酸酯快速搅拌均匀,倒入模具中自由发泡,泡沫体脱粘后脱模,放入电热鼓风干燥箱中,240℃固化1小时,制得聚氨酯-聚酰亚胺泡沫体。
测试泡沫的性能如下:
实施例5
本实施例提供一种阻尼层的制备:
阻尼涂层A组份的制备:
称取400克D-2000聚醚多元醇于1000ml三口瓶中,加热到100--110℃真空脱水1小时。降温到60℃以下,投入300克MDI-50多异氰酸酯,加热到80℃预聚反应2小时,出料置于密封容器中。取样测试游离异氰酸酯含量10%。
阻尼涂层B组份的制备:
称量下列各组分,于搅拌研磨分散机中研磨分散均匀制备B组份:
B组份以100质量份聚醚多元醇计:
聚醚多元醇:D-2000聚醚多元醇,100份。
胺扩链剂:二甲硫基甲苯二胺,30份。
硅烷偶联剂:γ-氨丙基三乙氧基硅烷(KH--550),12份。
受阻酚功能助剂:3,9-双{1,1-二甲基-2[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酰氧基]乙基}-2,4,6,8-四氧杂螺环-(5,5)十一烷(AO-80),35份。
阻尼填料:氢氧化铝,210份和云母粉,35份。
触变剂:有机膨润土,1.5份。
以A、B两组份按质量比为1:2配制阻尼涂层,涂层性能如下:
表干25℃ ≤6h,
实干25℃ ≤24h
与基材的黏结强度≥5Mpa。
自由阻尼损耗因子,平均Tanδ≥1.0。
实施例6
实施例1、2、3、4制备的聚氨酯-聚酰亚胺泡沫板作为芯材,芯材的上下表面涂敷2--3mm实施例5制备的阻尼涂层作为泡沫夹芯阻尼层,面材为在阻尼涂层上敷贴阻燃玻璃纤维布。芯材与面材之间构成约束阻尼复合结构泡沫夹芯材料,泡沫夹芯材料上下表面涂敷水性聚氨酯内舱涂料,作为外护装饰涂层。
由实施例1#、2#、3#、4#制备的吸声、阻尼泡沫夹芯复合材料性能列于表1中:
表1
Claims (3)
1.一种吸声阻尼泡沫夹芯复合材料,其特征在于,包括外层、内层和阻尼层,其中材料的外层为结构层;材料的内层为夹芯层,由开孔聚氨酯-聚酰亚胺泡沫组成;阻尼层位于外层与内层之间;
制备方法如下:聚氨酯-聚酰亚胺泡沫体作为芯材,表面涂布阻尼涂层,涂层外表面敷贴面材经室温或加温固化,制备具有吸声阻尼复合结构的泡沫夹芯材料。
2.根据权利要求1所述的复合材料,其特征在于,夹芯层的开孔聚氨酯-聚酰亚胺泡沫由下列重量份数的组分制成:
芳香二酐 100
极性溶剂 90~160
胺化物 15~30
脂肪醇 14~26
聚醚多元醇 25~35
泡沫稳定剂 1.0~3.5
催化剂 2~5
发泡剂 8~12
阻燃剂 30~50;
制备工艺为:
在备有搅拌器、温度计及回流冷凝器的三口瓶中,投入芳香二酐和极性溶剂,充分搅拌并缓慢升温,待固体芳香二酐全部溶解,加入胺化物反应至清澈溶液时,降温加入脂肪醇进行回流酯化反应,制得清澈透明二酸二酯溶液;降温到60℃以下,加入催化剂将溶液搅拌到恒温,制得前驱体溶液;
前驱体溶液按上述比例加入聚醚多元醇、泡沫稳定剂、催化剂、发泡剂、阻燃剂配制泡沫组合溶液;
泡沫组合溶液与异氰酸酯指数是1.0~1.05的多异氰酸酯快速搅拌均匀;倒入模具中自由发泡反应制得泡沫中间体,泡沫中间体脱粘后脱模,从模具中取出,放入微波炉或电热鼓风干燥箱中固化,制得聚酰亚胺泡沫体;
泡沫组合溶液与多异氰酸酯的重量比是100:100~105。
3.根据权利要求1所述的复合材料,其特征在于,阻尼层是一种聚醚型聚氨酯弹性体,由A、B两组份构成,A组份为异氰酸酯预聚体;B组份由聚醚多元醇、胺扩链剂、硅烷偶联剂、受阻酚功能助剂、阻尼填料、触变剂组成:
A组份异氰酸酯预聚体由聚醚多元醇和多异氰酸酯制备,两者的重量份数比是400:300;
制备方法如下:称取聚醚多元醇于1000ml三口瓶中,加热到100~110℃真空脱水1小时;降温到60~70℃,投入计量的多异氰酸酯,加热到80℃预聚反应2小时,出料置于密封容器中备用;
B组份的重量比:
聚醚多元醇100份;
胺扩链剂30份;
硅烷偶联剂12份;
受阻酚功能助剂35份;
阻尼填料245份;
触变剂1.5份;
制备方法如下:称量上述组分,于搅拌研磨分散机中研磨分散均匀制备B组份;
以A、B两组份按质量比1:2配制阻尼涂层。
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