CN108047698A - 一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料及其制备方法 - Google Patents
一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料及其制备方法 Download PDFInfo
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Abstract
一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料及其制备方法,涉及一种阻尼材料及其制备方法,利用溶液法制备掺杂有介孔分子筛的聚偏氟乙烯(PVDF)混合溶液,然后将其加入质量比为5:5的聚酯‑聚醚混合型聚氨醋(PU)预聚体中,再在交联剂作用下制备出介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。且由于与聚氨酯的部分互容性以及聚氨酯内部异氰酸根与多元醇构成的多相结构使材料具备更宽的阻尼温域,更重要的是由于介孔分子筛对分子链运动的束缚作用,使材料的阻尼峰值变高,此外该方法产品性能稳定,易工业化生产,可制备浇注型热固性弹性体、涂料及胶粘剂等产品。
Description
技术领域
本发明涉及一种阻尼材料及其制备方法,特别是涉及一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料及其制备方法。
背景技术
阻尼(damping或内耗)是指材料在振动中由于内部原因引起机械振动能消耗的现象,阻尼性能通常又称为减振性能,是材料的一种功能特性,从减振的角度上来看,就是将机械振动的量转化为热能或其他可以损耗的能量,从而达到减振的目的。近年来随着大型仪器设备的广泛应用,以及汽车、铁路工业的飞速发展,由此引起的噪声和振动问题变得尤为突出,并且机械振动会严重影响设备可靠性、稳定性和精度等,因此高性能阻尼材料的研发备受关注。
高分子基阻尼材料由于其在玻璃化转变温度附近具有很高阻尼因子,并且其结构可控性强,通过其制成高阻尼宽温域的阻尼材料将具有广阔的应用前景。单一的高分子阻尼材料的阻尼温域比较窄,不满足实际应用,采用两种或多种高分子材料共混可以有效解决这一问题。Qin C. L.等人则对聚氨酯/聚丙烯酸酯所形成的IPN体系进行了详细的研究,结果表明,极性或刚性的分子侧链对阻尼温域的提升有帮助,就阻尼温域来说,甲基丙烯酸丁酯>甲基丙烯酸乙酯>甲基丙烯酸甲酯>苯乙烯。Wu C. F. 等将受阻酚(AO-80)有机添加剂加入氯化聚乙烯、聚丙烯酸酯等聚合物当中,结果表明,随着AO-80含量的增加,tanδ的峰值向高温方向移动,并且tanδ峰值不断上升。中国专利CN102408701A公开了一种(PZT或PMN)加入热塑性聚氨醋中来提高材料阻尼性能,但其仍无法解决阻尼温域较窄的弊病。现实生活中,需要阻尼温域宽且阻尼峰值高的材料来满足实际应用。
发明内容
本发明的目的在于提供一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料及其制备方法,该方法采用聚酯-聚醚混合型聚氨酯拓宽阻尼温域,利用的PVDF压电性使机械振动更多的转化为电能,利用介孔分子筛对分子链运动的束缚作用提高材料的阻尼峰值,从而提高了材料的阻尼效果,产品性能稳定、易工业化生产,可制备浇注型热固性弹性体、涂料及胶粘剂等产品。
本发明的目的是通过以下技术方案实现的:
一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料,所述材料组成包括介孔分子筛、聚偏氟乙烯(PVDF)和聚酯-聚醚混合型聚氨酯(STPU);材料由质量比为5-30%介孔分子筛、10%-60%的PVDF和85%-10%的聚酯-聚醚混合型聚氨酯组成。
所述的一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料,所述聚酯-聚醚混合型聚氨酯是由聚酯型多元醇(聚四亚甲基醚二醇,PTMG)和聚醚型多元醇(聚已二酸乙二丙二醇酯,PEPA)构成的软段,由二苯基甲烷二异氰酸醋酯(MDI)和多亚甲基多苯基多异氰酸酯(TDI)构成的硬段。
一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料的制备方法,所述方法包括以下制备过程:
(1)PVDF和介孔分子筛混合溶液的制备:将经过60-80℃真空干燥6-12小时的PVDF溶于60-80℃的N,N-二甲基甲酰胺(DMF)溶剂中,然后将介孔分子筛加入PVDF溶液中,在60-80℃条件下混合1-3h,得到介孔分子筛掺杂PVDF混合溶液;
(2)聚氨酯预聚体的制备:将PTMG与TDI混合(异氰酸酯指数为1.00-1.05)在氮气保护条件下,温度70-85℃反应2-3小时,降温至室温后,制成聚醚型聚氨酯预聚体,分析NCO%的含量;另一方面将PEPA与MDI混合(异氰酸酯指数为1.00-1.05),同样在氮气保护条件下,温度70-85℃反应2-3小时,降温至室温后,制成聚酯型聚氨酯预聚体,分析NCO%的含量;
(3)将聚酯型聚氨酯预聚体和聚醚型聚氨酯预聚体按照质量比5:5混合,之后将介孔分子筛掺杂PVDF混合溶液放入混合型聚氨酯预聚体中,并将交联剂3,3'一二氯一4,4'一二氨基二苯基甲烷或二邻氯二苯胺甲烷(MOCA)以按照计算加入量,放入聚氨酯预聚体混合物中,在60-80℃充分搅拌条件下反应1-20分钟,之后倒入模具中,最后在90-100℃真空干燥3-12小时,制得介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
所述的一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料制备方法,所述方法制得的介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料需经极化处理,极化条件为极化温度80-100℃,极化电场2-10kv/mm,极化时间10-30分钟。
本发明的优点与效果是:
本发明的PVDF/STPU压电阻尼材料,由于PVDF与聚氨酯的部分互容性,以及聚氨酯内部聚酯-聚醚构成的多相结构使材料的阻尼温域达到100℃,利用介孔分子筛与聚合物间的摩擦提高材料的阻尼峰值,并且利用PVDF的压电性使机械振动更多的转化为了电能,在两者共同作用下提高了材料的阻尼效果,使材料的阻尼峰值达到以上1.0,且具有一定压电性,此外该方法产品性能稳定,易工业化生产,可制备浇注型热固性弹性体、涂料及胶粘剂等产品。
附图说明
图1为本发明制备过程流程图。
具体实施方式
下面结合实施例对本发明进行详细说明。
实施例1
首先将PVDF粉末真空烘箱中60℃条件下烘干12小时,然后在65℃条件下将干燥后的80gPVDF溶于100gDMF溶剂中,搅拌20分钟使PVDF完全溶解,然后将20g介孔分子筛(MCM-41)分2次逐步加入PVDF溶液中,边添加边搅拌,全部添加完毕后继续搅拌1小时,得到掺杂有介孔分子筛的PVDF混合溶液。
(1)将100g聚醚多元醇PTMG(羟值54.2mgKOH/g,分子量2000)加入脱水釜中,加热至100℃,真空脱水6小时,冷却至60℃,之后在氮气保护下,将9.8g已脱水的TDI(异氰酸酯指数为1.05,纯度90%)加入到预聚体反应器中,使温度升至80℃,反应2小时,降温至40℃,制得聚醚聚氨酯预聚体。
(2)将聚酯多元醇PEPA(羟值59.8mgKOH/g)加入脱水釜中,加热至110℃,真空脱水2小时,冷却至60℃,之后在氮气保护下,将17.2g已脱水的MDI(异氰酸酯指数为1.05,纯度90%)加入到预聚体反应器中,使温度升至80℃,反应2小时,降温至40℃,制得聚酯聚氨酯预聚体。
(3)分别取25g聚酯预聚体和25g聚醚预聚体放入同一个反应器中,在30℃条件下进行混合30分钟,然后将50g掺杂有介孔分子筛的PVDF混合溶液加入反应器中,加热混合预聚体至80℃,搅拌加入已经预熔好的MOCA7.2g,80℃充分搅拌条件下反应10分钟,之后倒入已经预热80℃的模具中,最后在100℃真空干燥6小时,制得介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
(4)将制得的样品在高压直流油浴装置中进行极化,极化条件为极化温度80℃,极化电场5Kv/mm,极化时间20分钟,即得极化后的介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
实施例2
(4)首先将PVDF粉末真空烘箱中80℃条件下烘干6小时,然后在65℃条件下将干燥后的50gPVDF溶于100gDMF溶剂中,搅拌20分钟使PVDF完全溶解,然后将10g介孔分子筛(MCM-41)分2次逐步加入PVDF溶液中,边添加边搅拌,全部添加完毕后继续搅拌1小时,得到掺杂有介孔分子筛的PVDF混合溶液。
(5)将100g聚醚多元醇PTMG(羟值54.2mgKOH/g,分子量2000)加入脱水釜中,加热至100℃,真空脱水6小时,冷却至60℃,之后在氮气保护下,将9.3g已脱水的TDI(异氰酸酯指数为1.05,纯度95%)加入到预聚体反应器中,使温度升至75℃,反应3小时,降温至30℃,制得聚醚聚氨酯预聚体。
(6)将聚酯多元醇PEPA(羟值59.8mgKOH/g)加入脱水釜中,加热至110℃,真空脱水2小时,冷却至60℃,之后在氮气保护下,将17.2g已脱水的MDI(异氰酸酯指数为1.05,纯度90%)加入到预聚体反应器中,使温度升至75℃,反应3小时,降温至30℃,制得聚酯聚氨酯预聚体。
(7)分别取20g聚酯预聚体和20g聚醚预聚体放入同一个反应器中,在30℃条件下进行混合30分钟,然后将60g掺杂有介孔分子筛的PVDF混合溶液加入反应器中,加热混合预聚体至80℃,搅拌加入已经预熔好的MOCA5.8g,80℃充分搅拌条件下反应5分钟,之后倒入已经预热80℃的模具中,最后在100℃真空干燥6小时,制得介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
(8)将制得的样品在高压直流油浴装置中进行极化,极化条件为极化温度90℃,极化电场3Kv/mm,极化时间20分钟,即得极化后的介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
实施例3
(9)首先将PVDF粉末真空烘箱中80℃条件下烘干6小时,然后在65℃条件下将干燥后的10gPVDF溶于40gDMF溶剂中,搅拌20分钟使PVDF完全溶解,然后将30g介孔分子筛(MCM-41)分2次逐步加入PVDF溶液中,边添加边搅拌,全部添加完毕后继续搅拌2小时,得到掺杂有介孔分子筛的PVDF混合溶液。
(10)将100g聚醚多元醇PTMG(羟值54.2mgKOH/g,分子量2000)加入脱水釜中,加热至100℃,真空脱水6小时,冷却至60℃,之后在氮气保护下,将9.3g已脱水的TDI(异氰酸酯指数为1.05,纯度95%)加入到预聚体反应器中,使温度升至70℃,反应2小时,降温至30℃,制得聚醚聚氨酯预聚体。
(11)将聚酯多元醇PEPA(羟值59.8mgKOH/g)加入脱水釜中,加热至110℃,真空脱水2小时,冷却至60℃,之后在氮气保护下,将17.2g已脱水的MDI(异氰酸酯指数为1.05,纯度90%)加入到预聚体反应器中,使温度升至70℃,反应2小时,降温至30℃,制得聚酯聚氨酯预聚体。
(12)分别取30g聚酯预聚体和30g聚醚预聚体放入同一个反应器中,在30℃条件下进行混合30分钟,然后将40g掺杂有介孔分子筛的PVDF混合溶液加入反应器中,加热混合预聚体至80℃,搅拌加入已经预熔好的MOCA8.7g,80℃充分搅拌条件下反应20分钟,之后倒入已经预热80℃的模具中,最后在100℃真空干燥8小时,制得介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
(13)将制得的样品在高压直流油浴装置中进行极化,极化条件为极化温度90℃,极化电场3Kv/mm,极化时间20分钟,即得极化后的介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
实施例4
(14)首先将PVDF粉末真空烘箱中80℃条件下烘干6小时,然后在60℃条件下将干燥后的10gPVDF溶于20gDMF溶剂中,搅拌20分钟使PVDF完全溶解,然后将5g介孔分子筛(MCM-41)逐步加入PVDF溶液中,边添加边搅拌,全部添加完毕后继续搅拌1小时,得到掺杂有介孔分子筛的PVDF混合溶液。
(15)将100g聚醚多元醇PTMG(羟值54.2mgKOH/g,分子量2000)加入脱水釜中,加热至100℃,真空脱水6小时,冷却至60℃,之后在氮气保护下,将9.3g已脱水的TDI(异氰酸酯指数为1.05,纯度95%)加入到预聚体反应器中,使温度升至70℃,反应2小时,降温至30℃,制得聚醚聚氨酯预聚体。
(16)将聚酯多元醇PEPA(羟值59.8mgKOH/g)加入脱水釜中,加热至110℃,真空脱水2小时,冷却至60℃,之后在氮气保护下,将17.2g已脱水的MDI(异氰酸酯指数为1.05,纯度90%)加入到预聚体反应器中,使温度升至70℃,反应2小时,降温至30℃,制得聚酯聚氨酯预聚体。
(17)分别取42.5g聚酯预聚体和42.5g聚醚预聚体放入同一个反应器中,在30℃条件下进行混合10分钟,然后将15g掺杂有介孔分子筛的PVDF混合溶液加入反应器中,加热混合预聚体至80℃,搅拌加入已经预熔好的MOCA12.3g,80℃充分搅拌条件下反应20分钟,之后倒入已经预热80℃的模具中,最后在100℃真空干燥8小时,制得介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
(18)将制得的样品在高压直流油浴装置中进行极化,极化条件为极化温度90℃,极化电场5Kv/mm,极化时间20分钟,即得极化后的介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
对比例1
市售聚氨酯减震垫(河北衡水振昌橡胶制品有限公司,型号DP80)
由表1可以看出实例1-4均具有较宽的阻尼温域,但是当组份中PVDF含量增高时其压电常数增加明显,最大压电常数达到18Cp/N,当材料中介孔分子筛含量增加时其损耗因子明显增大,最大值达到了1.23,综合实例1-4可以看出利用此种方法可以所制备出的压电阻尼复合材料具有优良的使用性能。
表1实施例1-4压电阻尼复合材料阻尼综合性能表
。
Claims (4)
1.一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料,其特征在于,所述材料组成包括介孔分子筛、聚偏氟乙烯(PVDF)和聚酯-聚醚混合型聚氨酯(STPU);材料由质量比为5-30%介孔分子筛、10%-60%的PVDF和85%-10%的聚酯-聚醚混合型聚氨酯组成。
2.根据权利1要求所述的一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料,其特征在于,所述聚酯-聚醚混合型聚氨酯是由聚酯型多元醇(聚四亚甲基醚二醇,PTMG)和聚醚型多元醇(聚已二酸乙二丙二醇酯,PEPA)构成的软段,由二苯基甲烷二异氰酸醋酯(MDI)和多亚甲基多苯基多异氰酸酯(TDI)构成的硬段。
3.一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料的制备方法,其特征在于,所述方法包括以下制备过程:
(1)PVDF和介孔分子筛混合溶液的制备:将经过60-80℃真空干燥6-12小时的PVDF溶于60-80℃的N,N-二甲基甲酰胺(DMF)溶剂中,然后将介孔分子筛加入PVDF溶液中,在60-80℃条件下混合1-3h,得到介孔分子筛掺杂PVDF混合溶液;
(2)聚氨酯预聚体的制备:将PTMG与TDI混合(异氰酸酯指数为1.00-1.05)在氮气保护条件下,温度70-85℃反应2-3小时,降温至室温后,制成聚醚型聚氨酯预聚体,分析NCO%的含量;另一方面将PEPA与MDI混合(异氰酸酯指数为1.00-1.05),同样在氮气保护条件下,温度70-85℃反应2-3小时,降温至室温后,制成聚酯型聚氨酯预聚体,分析NCO%的含量;
(3)将聚酯型聚氨酯预聚体和聚醚型聚氨酯预聚体按照质量比5:5混合,之后将介孔分子筛掺杂PVDF混合溶液放入混合型聚氨酯预聚体中,并将交联剂3,3'一二氯一4,4'一二氨基二苯基甲烷或二邻氯二苯胺甲烷(MOCA)以按照计算加入量,放入聚氨酯预聚体混合物中,在60-80℃充分搅拌条件下反应1-20分钟,之后倒入模具中,最后在90-100℃真空干燥3-12小时,制得介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料。
4.根据权利要求3所述的一种介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料制备方法,其特征在于,所述方法制得的介孔分子筛掺杂聚偏氟乙烯/聚氨酯压电阻尼材料需经极化处理,极化条件为极化温度80-100℃,极化电场2-10kv/mm,极化时间10-30分钟。
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