CN102639620A - 含有微珠的树脂泡沫 - Google Patents
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Abstract
本发明涉及一种包含微珠且用于吸声的泡沫,该泡沫包含相对于聚合物泡沫和微珠的总重量为40-85重量%开孔聚合物泡沫和15-60重量%具有柔性外层的微珠,其中该微珠的D50值为至少70微米且不大于250微米,以及一种生产所述泡沫的方法,该方法包括如下步骤:I)用包含可发泡微珠的液态分散体浸渍开孔聚合物泡沫,II)任选地,压制/压缩和/或干燥聚合物泡沫,和III)在高于可发泡微珠的发泡温度且低于其分解温度的温度下热处理经浸渍的聚合物泡沫以使微珠发泡。
Description
本发明涉及一种用于吸声的包含具有柔性外层的中空微珠的开孔泡沫,其中所述中空微珠的D50值为至少70μm且至多250μm,以及一种生产所述开孔泡沫的方法及其在吸声和/或绝热中的用途。
现代社会对用于吸声和隔音的材料要求严格。吸声和隔音材料用于改善立体声效果,例如降低不希望的混响程度。为此通常使用塑料,这些材料由于具有优异的粘弹性、易于加工和可商购获得而为合适的材料。这些塑料的使用形式通常为多孔泡沫形式。
多孔材料的特征在于其在高频率下显示出良好吸声,但在较低频率下具有低吸收能力。塑料泡沫在较低频率下的吸声可例如通过使用薄膜和层(振动)或通过使用共振器而改善。然而,这些措施效果有限,因为频率范围收到限制,而且还由于结构限制如宽度和重量。
改善塑料隔音和吸声性能的另一可能性为将各种填料引入塑料中。
US5,378,733描述了用于减小声音的聚氨酯组合物,所述组合物包含双组分聚氨酯粘合剂、密度高于5的颗粒状填料和作为第二种填料的密度低于0.5的中空聚合物微珠。将所述中空微珠在使各组分反应以获得聚氨酯之前通过在多元醇组分中分散而引入。
WO2004/022298A1涉及一种声学隔断材料,该材料通过热塑性橡胶颗粒和PU塑料颗粒的挤出而生产,其中加入可发泡中空体作为发泡剂。
WO98/52997A1公开了一种由环氧树脂和热塑性材料的混合物制成的泡沫。可使用的发泡剂尤其为可热发泡的中空微珠。WO98/52997中描述的泡沫尤其可在汽车中用作隔音元件。
US5,272,001涉及开孔柔性聚氨酯泡沫,为了改善弹性和震动吸收性能,其包含平均直径为35-60μm的中空微珠。
尽管迄今为止公开了改性泡沫,但仍需要在相对低频率范围内具有改善的吸声和隔音性能的泡沫。
本发明通过包含中空微珠且用于吸声的泡沫实现该目的,所述泡沫基于聚合物泡沫和中空微珠的总重量包含:
40-85重量%开孔聚合物泡沫,和
15-60重量%具有柔性外层的中空微珠,其中所述中空微珠的D50值为至少70μm且至多250μm。
在约300-1600Hz的频率范围中,本发明泡沫与不包含或包含较低量中空微珠的相同泡沫相比具有较高的吸声系数。令人惊讶地,泡沫中所包含的中空微珠的效果取决于其尺寸。中空微珠必须具有最小尺寸从而产生有利的效果,即所需吸声性能的改善。D50值为约35-55μm的中空微珠对泡沫吸声没有影响,但不同的是如果泡沫包含D50值≥70μm的较大中空微珠,则它们显示出较高吸声系数和较高流阻,这同样与隔音效果的改善有关。令人惊讶地,尽管必须使用相对大的中空微珠,但中空微珠的存在对本发明泡沫的机械性能没有或仅具有非常轻微的不利影响。
下文对本发明进行详细描述。
本发明泡沫包含基于开孔聚合物泡沫和中空微珠的总重量为40-85重量%,优选50-80重量%的开孔聚合物泡沫。
开孔泡沫为其中泡沫结构基本上由大量相互连接的三维支化泡孔壁构成的那些。由聚合物膜密封的开孔聚合物泡沫的面积越小,泡沫的弹性就越大。
优选使用本发明开孔聚合物泡沫,所述泡沫包含大量相互连接的三维支化泡孔壁,其中壁的平均长度与厚度之比大于10:1,优选大于12:1,尤其是大于15:1,并且其中壁的密度大于1.1g/cm3,优选大于1.2g/cm3,尤其是大于1.3g/cm3。
平均长度与厚度之比以显微镜测定且本文中壁的长度和厚度通过统计评价方法测定。本文中壁的长度定义为两个连接点中心之间的距离且本文中壁的厚度定义为壁的最窄点处的厚度,在每种情况下在显微照片上测量。为了测定泡沫中壁的密度,将泡沫置于合适的液体中,用所述液体使其借助其开孔性质而完全饱和,液体实例为异丙醇。然后使用阿基米德原理测定泡孔壁的密度。
在本发明中,优选开孔聚合物泡沫为弹性的。
弹性泡沫在变形后具有高回弹力。称为弹性泡沫的泡沫尤其为当经受根据DIN 53580的压缩变形至其50%厚度时,不显示出大于其起始体积的2%的残留变形的那些(Chemie-Lexikon [化学百科全书],1995年第9版,第4016页)。
原则上,聚合物泡沫可以由本领域技术人员已知的适于生产开孔聚合物泡沫的任意聚合物生产。优选该聚合物泡沫选自热固性泡沫,尤其优选选自苯酚-甲醛树脂泡沫、脲-甲醛树脂泡沫和蜜胺-甲醛树脂泡沫,特别优选蜜胺-甲醛树脂泡沫。
合适蜜胺-甲醛树脂泡沫的生产例如描述于EP0017671B1中,且合适脲-甲醛树脂泡沫例如由EP0031513B1已知。可用于本发明中的热固性泡沫如苯酚-甲醛树脂泡沫的生产例如描述于EP0049768B1中。
开孔泡沫的包封密度通常为5-100g/l,优选8-20g/l。拉伸强度优选为100-150kPa,其中断裂拉伸强度为8-20%。
本发明泡沫包含15-60重量%,优选20-50重量%具有柔性外层的中空微珠,其中所述中空微珠的D50值为至少70μm且至多250μm。
所述中空微珠具有柔性外层,这意味着中空微珠易于压缩,且具有足以经受多次负载循环或压力循环而不使其壳破裂的弹性。优选使用具有由一种或多种均聚物和/或一种或多种共聚物形成的外层的中空微珠,其中这些的玻璃化转变温度低于泡沫的使用温度。特别优选中空微珠的外层由一种或多种热塑性均聚物和/或共聚物形成。
非常优选本发明泡沫中所包含的中空微珠为已通过可发泡中空微珠的发泡而获得的已发泡中空微珠。该类型的中空微珠基本上由不漏气的聚合物外层和包覆于其中的液态或气态发泡剂构成。可发泡和相应的已发泡中空微珠的外层通常类似于热塑性材料,从而允许可发泡中空微珠在发泡剂因受热而发泡时软化并发泡。外层所用均聚物和/或共聚物可为线性、支化或交联的聚合物。外层通常使用包含丙烯酸、甲基丙烯酸、苯乙烯、偏氯乙烯、丙烯腈、甲基丙烯腈等或其混合物的聚合物和共聚物。所用发泡剂通常包含低级烃如丙烷、正丁烷、异丁烷、异戊烷、正戊烷、新戊烷、己烷、庚烷和石油醚,以及卤化烃如氯甲烷、二氯甲烷、三氯一氟甲烷和二氯二氟甲烷。可发泡中空微珠可以由已知方法如US 3,615,972所述那些生产。可发泡中空微珠的平均直径通常在发泡后增大4-6倍。
在本发明中,泡沫中所包含的中空微珠的D50值为至少70μm,优选至少90μm,非常特别优选至少100μm。D50值为50%颗粒的直径较小或50%颗粒的直径较大的颗粒直径。D50值可例如借助光散射测定。测定D50值的方法的实例描述于Akzo Nobel的Technical Bulletins No.3B中。
在本发明中,优选泡沫中所包含的中空微珠的D50值为至多250μm。所述中空微珠用于填充泡沫孔隙的体积,但不堵塞泡沫的孔隙和通道。
在本发明中,优选中空微珠的位置处于开孔聚合物泡沫的孔隙内。
本发明进一步提供了一种生产包含中空微珠的泡沫的方法,尤其是生产包含上述中空微珠的泡沫的方法,所述方法包括如下步骤:
I)用包含可发泡中空微珠的液态分散体浸渍开孔聚合物泡沫,
II)合适的话,压制/压缩和/或干燥所述聚合物泡沫,和
III)在高于可发泡中空微珠的发泡温度且低于其分解温度的温度下热处理经浸渍的聚合物泡沫以使中空微珠发泡。
在步骤I)中,用包含可发泡中空微珠的液态分散体浸渍开孔聚合物泡沫。浸渍可用包含可发泡中空微珠的分散体经由喷雾施加或浸没和饱和进行,例如通过初湿含浸法(incipient-wetness method),其中聚合物泡沫的孔隙体积由近似相同体积的浸渍溶液填充并干燥载体。还可用过量溶液操作,其中所述溶液的体积大于聚合物泡沫的孔隙体积。本文中使聚合物泡沫与浸渍溶液混合并搅拌足够时间。
用于浸渍方法的混合物包含基于液态分散体的总重量为0.01-50重量%,优选1-10重量%的可发泡中空微珠和50-99.99重量%,优选90-99重量%的液态分散介质。用于浸渍方法的混合物的浓度和量由本领域技术人员调节至适于待浸渍的聚合物泡沫和包含中空微珠的泡沫的所需构造。例如具有低浓度中空微珠的浸渍混合物用于低密度聚合物泡沫。
用于浸渍方法的可发泡中空微珠的D50值优选>16μm,优选>20μm,特别优选>25μm。为了确保将中空微珠均匀掺入孔隙空间而不阻塞孔隙和通道,优选使用D50值≤100μm,特别优选≤50μm的中空微珠,在每种情况下基于发泡方法之前的尺寸。
所用分散介质优选包含水和/或C1-C4醇,并且这特别适用于其中聚合物泡沫选自极性聚合物的情况,非常特别是其中聚合物泡沫选自蜜胺-甲醛树脂泡沫、脲-甲醛树脂泡沫和苯酚-甲醛树脂泡沫的情况。
用于浸渍方法的混合物可包含其他组分,其实例为:
a)用于疏水化的含氟烃树脂(参见WO2008/037600)
b)疏水化和阻燃物质(参见WO2007/023118)。
合适的话,将浸渍的聚合物泡沫在步骤II)中压制或压缩并干燥,这优选在低于可发泡中空微珠发泡温度的温度下进行。
压制方法可以例如如EP0451535A所述进行,通过使泡沫通过在两个反向旋转的平行辊之间的确定狭缝中压制。
除使泡沫通过两个反向旋转辊之间的狭缝外,另一种可能性是通过通过在传送带上运输经浸渍的泡沫并将以与泡沫运动相同的圆周速率旋转的辊压在泡沫上而施加必要的压力。在对泡沫施加压力的另一方法中,将泡沫例如置于撞击压制泡沫的压制机中。然而,在这种情况下,连续压制是不可能的。
在本发明方法的步骤III)中,在高于可发泡中空微珠的发泡温度且低于中空微珠的分解温度的温度下热处理经浸渍的聚合物泡沫使得中空微珠发泡。准确的热处理温度取决于所用的可发泡中空微珠以及热处理时间。
以上对包含中空微珠的本发明泡沫所述的生产方法的优点在于其能确保保留所用开孔聚合物泡沫的结构。在发泡方法之前较小的中空微珠在浸渍步骤中均匀分布于聚合物泡沫孔隙内并在孔隙内发泡。由于本发明使用具有柔性外层的中空微珠,在发泡方法后中空微珠还可以完全填充各孔隙而不破坏聚合物泡沫的结构,这是因为所述微珠可以使其本身适合各孔隙。
本发明还提供了上述包含中空微珠的泡沫在吸声、隔音和绝热,尤其是在机动车辆建造、有轨交通工具建造、造船和飞机建造中以及在太空中的用途。本发明还提供了吸声和绝热元件,该元件包含上述泡沫,其实例为墙板和天花板。
下文实施例用于说明本发明。
实施例
实施例1(本发明)
将蜜胺-甲醛树脂泡沫(G,密度为7.3g/l,BASF SE)用可发泡中空微珠的水溶液饱和。该中空微珠为Akzo Nobel的091DU140。珠外层由丙烯酸酯、偏氯乙烯和丙烯腈的共聚物构成。中空微珠包含包覆的发泡剂(异丁烷或异戊烷)。根据生产商的信息,可发泡颗粒的D50值为35-45μm。将经浸渍的聚合物泡沫在100°C下于烘箱中干燥,然后在130°C下1小时,此时中空微珠发泡至约100-150μm的尺寸。
实施例2(对比)
实施例3测量吸声系数
根据ISO 10534-2测定来自实施例1和2的用中空微珠浸渍的聚合物泡沫的吸声。表1给出实施例1的结果且表2给出实施例2的结果。
表1来自实施例1(本发明)的聚合物泡沫的吸收系数
表2来自实施例2(对比)的负载有中空微珠的聚合物泡沫的吸收系数
实施例4测量流阻
测定来自实施例1和2的包含中空微珠的聚合物泡沫的ISO 9053流阻。表3和4列出了结果。
表3实施例1(本发明)泡沫的流阻
中空微珠的浓度[重量%] | 密度[g/l] | 流阻*[Pa*s/m2] |
0 | 7.3 | 11850 |
10 | 8.1 | 13225 |
20 | 8.5 | 17225 |
30 | 8.7 | 20425 |
在30%负载下,与标准相比流阻几乎翻倍。
表4实施例2(对比)泡沫的流阻
中空微珠的浓度[重量%] | 密度[g/l] | 流阻*[Pa*s/m2] |
0 | 7.3 | 11700 |
5 | 8.3 | 10725 |
7 | 8.2 | 11675 |
25 | 8.7 | 11925 |
用较小的Expancel SL40微珠饱和的Basotect没有改善吸收或流阻。因此,珠的尺寸对声学性能具有显著影响。
Claims (11)
1.一种包含中空微珠且用于吸声的泡沫,其基于聚合物泡沫和中空微珠的总重量包含:
40-85重量%开孔聚合物泡沫,和
15-60重量%具有柔性外层的中空微珠,其中所述中空微珠的D50值为至少70微米且至多250微米。
2.根据权利要求1的泡沫,其中所述开孔聚合物泡沫的密度为5-100g/l。
3.根据权利要求1或2的泡沫,其中所述聚合物泡沫选自苯酚-甲醛树脂泡沫、脲-甲醛树脂泡沫和蜜胺-甲醛树脂泡沫,优选蜜胺-甲醛树脂泡沫。
4.根据权利要求1-3中任一项的泡沫,其中所述中空微珠的外层由一种或多种玻璃化转变温度低于泡沫使用温度的均聚物和/或共聚物形成。
5.根据权利要求1-4中任一项的泡沫,其中所述中空微珠的D50值≥90微米。
6.一种生产根据权利要求1-5中任一项的包含中空微珠的泡沫的方法,包括如下步骤:
I)用包含可发泡中空微珠的液态分散体浸渍开孔聚合物泡沫,
II)合适的话,压制/压缩和/或干燥所述聚合物泡沫,和
III)在高于可发泡中空微珠的发泡温度且低于其分解温度的温度下热处理经浸渍的聚合物泡沫以使中空微珠发泡。
7.根据权利要求6的方法,其中用于浸渍方法的可发泡中空微珠的D50值>16微米且≤100μm,优选≤50μm。
8.根据权利要求6或7的方法,其中在步骤I)中用于浸渍方法的混合物包含基于液态分散体总重量为0.01-50重量%的可发泡中空微珠和50-99.99重量%的液态分散介质。
9.根据权利要求6-8中任一项的方法,其中在步骤I)使用水和/或C1-C4醇作为分散介质。
10.根据权利要求1-5中任一项的包含中空微珠的泡沫在吸声和/或绝热中的用途。
11.一种包含根据权利要求1-5中任一项的包含中空微珠的泡沫的吸声和/或绝热元件。
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US20110237694A1 (en) | 2010-03-23 | 2011-09-29 | Basf Se | Polyarylene ethers with improved flowability |
US20110237693A1 (en) | 2010-03-23 | 2011-09-29 | Basf Se | Blends made of polyarylene ethers and of polyarylene sulfides |
US20110237699A1 (en) | 2010-03-24 | 2011-09-29 | Basf Se | Process for producing molded foams from melamine/formaldehyde condensation products |
WO2011117344A1 (de) | 2010-03-24 | 2011-09-29 | Basf Se | Nachvernetzte polyamide und verfahren zu deren herstellung |
US20120088048A1 (en) | 2010-04-01 | 2012-04-12 | Basf Se | Process for producing fiber-reinforced composite materials |
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US20110288258A1 (en) | 2010-05-19 | 2011-11-24 | Basf Se | Crosslinked polyamide |
US8703862B2 (en) | 2010-05-26 | 2014-04-22 | Basf Se | Reinforced thermoplastic molding compositions based on polyarylene ethers |
US20120071578A1 (en) | 2010-09-16 | 2012-03-22 | Basf Se | Producing melamine-formaldehyde foams |
US9242397B2 (en) | 2010-11-05 | 2016-01-26 | Basf Se | Melamine resin foam with inorganic filling material |
US8937106B2 (en) | 2010-12-07 | 2015-01-20 | Basf Se | Melamine resin foams with nanoporous fillers |
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- 2010-11-16 CN CN201080052601.7A patent/CN102639620B/zh not_active Expired - Fee Related
- 2010-11-16 US US13/510,487 patent/US9056961B2/en not_active Expired - Fee Related
- 2010-11-16 EP EP10779788.8A patent/EP2501749B1/de not_active Not-in-force
- 2010-11-16 ES ES10779788T patent/ES2435811T3/es active Active
- 2010-11-16 WO PCT/EP2010/067556 patent/WO2011061178A1/de active Application Filing
- 2010-11-16 KR KR1020127015841A patent/KR20120117784A/ko active IP Right Grant
- 2010-11-16 JP JP2012539299A patent/JP5538556B2/ja not_active Expired - Fee Related
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106661250A (zh) * | 2014-04-30 | 2017-05-10 | 皮特·卡德尔 | 涂覆泡沫方法和设备 |
CN106082910A (zh) * | 2016-06-13 | 2016-11-09 | 南通南京大学材料工程技术研究院 | 一种可瓷化柔性保温饰面砖及其制备方法 |
CN109318552A (zh) * | 2018-05-30 | 2019-02-12 | 桑德(上海)建筑科技有限公司 | 一种吸音载体开孔颗粒聚合板及其制备方法 |
CN109318552B (zh) * | 2018-05-30 | 2021-12-28 | 桑德(上海)建筑科技有限公司 | 一种吸音载体开孔颗粒聚合板及其制备方法 |
CN111635551A (zh) * | 2020-06-23 | 2020-09-08 | 哈尔滨工程大学 | 一步法制备聚酰亚胺开孔泡沫的方法及产品 |
CN111635551B (zh) * | 2020-06-23 | 2022-04-22 | 哈尔滨工程大学 | 一步法制备聚酰亚胺开孔泡沫的方法及产品 |
Also Published As
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JP2013511583A (ja) | 2013-04-04 |
CN102639620B (zh) | 2014-01-22 |
WO2011061178A1 (de) | 2011-05-26 |
ES2435811T3 (es) | 2013-12-23 |
EP2501749A1 (de) | 2012-09-26 |
US9056961B2 (en) | 2015-06-16 |
KR20120117784A (ko) | 2012-10-24 |
US20120225965A1 (en) | 2012-09-06 |
JP5538556B2 (ja) | 2014-07-02 |
EP2501749B1 (de) | 2013-09-18 |
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