CN107057011A - 抗老化和低排放的床垫和/或坐垫 - Google Patents
抗老化和低排放的床垫和/或坐垫 Download PDFInfo
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- CN107057011A CN107057011A CN201710071028.8A CN201710071028A CN107057011A CN 107057011 A CN107057011 A CN 107057011A CN 201710071028 A CN201710071028 A CN 201710071028A CN 107057011 A CN107057011 A CN 107057011A
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- foam
- mattress
- cushion
- polyurethane foams
- din
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- 150000002978 peroxides Chemical class 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000011548 physical evaluation Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000011495 polyisocyanurate Substances 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 description 1
- VAKMIIPDYZXBEV-DPMBMXLASA-M potassium;(z,12r)-12-hydroxyoctadec-9-enoate Chemical compound [K+].CCCCCC[C@@H](O)C\C=C/CCCCCCCC([O-])=O VAKMIIPDYZXBEV-DPMBMXLASA-M 0.000 description 1
- RLEFZEWKMQQZOA-UHFFFAOYSA-M potassium;octanoate Chemical compound [K+].CCCCCCCC([O-])=O RLEFZEWKMQQZOA-UHFFFAOYSA-M 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 150000003140 primary amides Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
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- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 150000003334 secondary amides Chemical class 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- 238000010998 test method Methods 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- VNTDZUDTQCZFKN-UHFFFAOYSA-L zinc 2,2-dimethyloctanoate Chemical compound [Zn++].CCCCCCC(C)(C)C([O-])=O.CCCCCCC(C)(C)C([O-])=O VNTDZUDTQCZFKN-UHFFFAOYSA-L 0.000 description 1
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- PVLBCXWFQZZIGP-UHFFFAOYSA-L zinc;nonanoate Chemical compound [Zn+2].CCCCCCCCC([O-])=O.CCCCCCCCC([O-])=O PVLBCXWFQZZIGP-UHFFFAOYSA-L 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
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Abstract
本申请描述了包含至少一个区段的软质聚氨酯泡沫的抗老化和低排放的床垫和/或坐垫,其中所述软质聚氨酯泡沫已通过在式(I)化合物和至少一种发泡剂存在下使至少一种多元醇组分和至少一种异氰酸酯组分反应而获得。
Description
技术领域
本发明属于床垫和/或坐垫,特别是床垫以及软质聚氨酯泡沫的领域。本发明优选涉及提供床垫和/或坐垫,特别是床垫,其包括至少一个由软质聚氨酯泡沫构成的区段(section)。
背景技术
含有聚氨酯泡沫的床垫和/或坐垫从现有技术公知已久,并且在全世界被采用。从不缺乏对此类床垫和/或坐垫进行改进的尝试,以例如使最佳的睡眠舒适性成为可能。到目前为止,对优化的需要尚未完全得到满足。
在含有聚氨酯泡沫的床垫和/或坐垫领域中不断发生的问题一直是老化行为。在老化过程中,材料疲劳可发生在床垫和/或坐垫中。这里,例如,床垫和/或坐垫的硬度可局部地改变或分布在整个床垫上。在多数情况下,观察到硬度的降低。这可导致整个床垫上形成睡眠中空或硬度差异。差的床垫常常引起背部问题、头痛或睡眠紊乱。
材料疲劳的主要原因是床垫和/或坐垫在放置时的压缩。床垫材料中的热、湿气、UV辐射以及氧化和降解过程同样可加速材料疲劳的过程。这特别适用于含有软质聚氨酯泡沫的床垫和/或坐垫。特别是当使它们经受热(热老化)时,所使用的聚氨酯泡沫的抗热性和/或抗老化性仍需要进一步改进。叔胺通常用作此类软质PU泡沫生产中的催化剂,特别是为了催化异氰酸酯和多元醇之间以及异氰酸酯和水之间的反应。因此,此类化合物可有效地被视为用于生产软质PU泡沫的必要添加剂。然而,这些胺催化剂中的许多通常对PU泡沫的抗老化性有不利影响。与含有聚氨酯泡沫的床垫和/或坐垫相关的又一问题是这些产品的排放特征必须满足有时苛刻的要求。胺排放经常对总排放特征起主要作用。进而,柔软聚氨酯泡沫的比例在多数情况下导致这些含有聚氨酯泡沫的床垫和/或坐垫的胺排放。因此,生产低排放和抗老化的软质聚氨酯泡沫作为含有聚氨酯泡沫的床垫和/或坐垫的组分仍然是常见的挑战。
鉴于该背景,本发明的具体目的是提供具有特别低的胺排放量且同时具有特别良好的抗老化性的含有聚氨酯泡沫的床垫和/或坐垫。
出于本发明的目的,有关胺的“低排放”特别意指用于生产床垫和/或坐垫、优选用于生产床垫的软质聚氨酯泡沫具有≥0μg/m3至≤40μg/m3、优选≤10μg/m3、特别优选≤5μg/m3的胺排放,如通过基于DIN标准DIN EN ISO 16000-9:2008-04的试验室方法、在加载测试室后24小时适当地确定。
出于本发明的目的,“抗老化”特别意指软质聚氨酯泡沫的老化行为、特别是耐热性和/或在加热(热老化)时的抗老化性的改进。此类老化现象通常与用于生产软质聚氨酯泡沫的催化剂体系的选择密切相关,并且通常会导致材料疲劳。
发明内容
在本发明的上下文中,已惊奇地发现,该目的可通过本发明的主题来实现。本发明提供了包含至少一个区段的软质聚氨酯泡沫的床垫和/或坐垫,其中所述软质聚氨酯泡沫已通过在式(I)化合物和至少一种发泡剂存在下使至少一种多元醇组分和至少一种异氰酸酯组分反应而获得:其它常规添加剂、活性材料和助剂当然也可任选地有利地用于上述反应中。出于本发明的目的,非常特别优选的是床垫。这也有利地适用于下面的所有优选实施方案。
以这种方式使用式(I)化合物生产的软质聚氨酯泡沫在胺排放方面有利地特别低,并且同时特别抗老化,如可特别地借助于如实施例中所示的测试方法所验证的。与使用根据现有技术的常规催化剂生产的软质聚氨酯泡沫相比,当使用式(I)的本发明的含氮化合物时,可有利地改进相应的软质聚氨酯泡沫的抗热性和/或耐久性。在特别是软质聚氨酯泡沫、优选软质块料(slabstock)泡沫的情况下,特别是在根据DIN标准的DIN EN ISO2440/A1:2009-01的干热老化的情况下,特别是在70℃、100℃、120℃、125℃和/或140℃的温度以及2小时、4小时、16小时、22小时、24小时、48小时、72小时和/或168小时,优选2小时、24小时和/或168小时的老化时间下,可有利地观察到该积极效果。
床垫本身和其生产是已知的。它们通常由床垫芯和围绕所述床垫的覆盖物组成,所述床垫芯包括例如泡沫、乳胶、天然产品和/或弹簧芯。相应的情况适用于坐垫。至少一段软质聚氨酯泡沫存在于床垫和/或坐垫中的陈述意味着所述床垫和/或所述衬垫的至少一部分由软质聚氨酯泡沫或各种软质聚氨酯泡沫组成。基于床垫和/或坐垫的总重量,该部分可占至少1重量%或5重量%或25重量%,优选至少50重量%,特别是至少75重量%。除了覆盖物之外,床垫和/或坐垫还可以完全由软质聚氨酯泡沫组成。
聚氨酯泡沫的生产同样是已知的。其通过在至少一种发泡剂(例如水)存在下使至少一种多元醇组分和至少一种异氰酸酯组分在加聚反应中的试验和测试过的反应而形成。这里对于本发明重要的是,在式(I)化合物存在下实施该反应:
根据本发明的优选实施方案,存在于床垫和/或坐垫中的软质聚氨酯泡沫是热固化的软质聚氨酯泡沫、高回弹性软质聚氨酯泡沫或粘弹性软质聚氨酯泡沫,或使用这些软质泡沫的组合,例如,这些软质泡沫中的两种或三种的组合。上述软质泡沫类型之间的区别本身是本领域技术人员已知的;这些是已在本领域中相应建立的众所周知的技术术语,但仍将在此加以简要解释。
高回弹性软质泡沫和热固化的软质泡沫之间的关键差异在于在前一种情况下使用高反应性多元醇以及任选存在的低分子量交联剂,其中所述交联剂的功能还能够通过相对高官能度的异氰酸酯来实现。异氰酸酯基团与羟基的反应因此早在泡沫的膨胀阶段(由–NCO和H2O形成CO2)中发生。因此,由于粘度增加,这种快速的聚氨酯反应通常导致在发泡过程期间泡沫的相对高的固有稳定性。高回弹性软质聚氨酯泡沫通常是高弹性泡沫,其中外部区域的稳定化起巨大作用。由于高的固有稳定性,因此泡孔通常在发泡过程结束时仍未充分打开,它们必须另外被机械地破开。这里所需的力(“压碎力”(FTC))是开孔比例的量度。通常期望具有高比例的仅需低压碎力的开孔泡沫。在模具中发泡时,与热固化的软质聚氨酯泡沫相比,高回弹性软质聚氨酯泡沫是在例如≤90℃的温度下生产的。
开孔软质聚氨酯泡沫通常具有在1至250mm水柱范围内,特别是在1至50mm水柱范围内的透气率(也称为“孔隙率”)(优选其通过测量通过泡沫样本发生流动时的压力差来确定)。为此,将5cm厚的泡沫盘置于光滑的基底上。将800g重量(10cm x 10cm)和中孔(直径2cm)以及软管连接的板置于泡沫板上。通过中孔,使8l/min的恒定空气流通入泡沫样本中。泡沫越封闭,累积压力越多,水柱的表面被向下压迫就越多,测量值就越大。
取决于应用,热固化的软质泡沫通常具有在8至80kg/m3范围内的泡沫密度。特别是用于生产高质量床垫的高回弹性软质泡沫通常在25-80kg/m3的密度范围内被生产。这里,当使用此类泡沫作为床垫、床垫组件和/或坐垫时,特别要根据消费者的区域情况、要求和偏好进行区分。
高回弹性软质泡沫的关键特征是回弹性(rebound resilience)(也称为“落球回弹(ball rebound)”(BR)或“回弹(resilience)”)。确定回弹性的方法描述于例如DIN ENISO 8307:2008-03中。这里,使具有固定质量的钢球从特定高度落到测试样本上,然后测量以下落高度的百分数%表示的回弹高度。高回弹性软质泡沫的典型值通常在≥55%的范围内。因此,高回弹性软质泡沫经常也被称为HR泡沫。相比之下,热固化的软质聚氨酯泡沫具有通常15%至最大60%的回弹值。
一种特殊类型的聚氨酯泡沫是粘弹性泡沫类。这些也被称为“记忆泡沫”,并展示低回弹性(优选<10%)以及压缩后的缓慢逐渐恢复(恢复时间优选2-10s)两者。这种材料在现有技术中是众所周知的,并且特别由于它们的吸能和吸声性质而非常有价值。与常规的软质聚氨酯泡沫相比,典型的粘弹性泡沫通常具有低孔隙率和高密度(或高泡沫密度(FD))。坐垫具有通常30-50kg/m3的泡沫密度,因此在粘弹性泡沫典型的密度标度的下端,而床垫通常具有在60-130kg/m3范围内的密度。
在常规的聚氨酯泡沫中,硬(高玻璃化转变温度)相和软(低玻璃化转变温度)相在聚合期间变得彼此相邻排布,然后自发地彼此分离,以在“本体聚合物”内形成形态上不同的相。此类材料也被称为“相分离”材料。在这种情况下,粘弹性聚氨酯泡沫是其中仅仅不完全地(如果有的话)发生上述相分离的特殊情况。在粘弹性泡沫的情况下,玻璃化温度优选在-20至+15℃的范围内,而相比之下,热固化的软质聚氨酯泡沫和高回弹性软质聚氨酯泡沫的玻璃化转变温度通常低于-35℃。主要基于聚合物的玻璃化温度的这种“结构粘弹性”应当与具有(主要)开孔的聚氨酯泡沫的归因于气动效应的粘弹性区别开。这是因为在后一种情况下,在泡沫材料内存在实质上闭合的孔,即仅略微打开的孔。由于孔口的小尺寸,因此空气在压缩之后仅仅逐渐回流,这导致减慢的恢复。
各种软质聚氨酯泡沫不仅根据泡沫密度,而且通常还根据它们的压缩强度(也称为承载能力)来进行用于特定应用的分类。因此,热固化的软质聚氨酯泡沫根据DIN EN ISO3386-1:2015-10的40%的压缩强度CLD(压缩载荷变形)通常在2.0-8.0kPa的范围内。高回弹性软质泡沫通常具有2.0至5.0kPa、特别是2.5至4.5kPa的值,而粘弹性聚氨酯泡沫通常具有0.1-5.0kPa、特别是0.5-2.0kPa的值。
在本发明的一个优选实施方案中,将要根据本发明使用的软质聚氨酯泡沫在回弹性、泡沫密度和/或孔隙率方面具有以下优选的性质(任选在压开泡沫之后,特别是在高回弹性软质聚氨酯泡沫的情况下),即根据DIN EN ISO 8307:2008-03测量的1%至80%的回弹性、和/或5至150kg/m3的泡沫密度、和/或1至250mm水柱、特别是1至50mm水柱的孔隙率。特别优选满足如上所示的关于回弹性、泡沫密度和/或孔隙率的所有3个准则。特别地,根据本发明使用的软质聚氨酯泡沫具有0.1至8.0kPa的根据DIN EN ISO 3386-1:2015-10的压缩强度CLD 40%。
热固化的软质聚氨酯泡沫、高回弹性软质聚氨酯泡沫和粘弹性软质聚氨酯泡沫和其制备本身是已知的。出于本发明的目的,热固化的软质聚氨酯泡沫特别具有2.0-8.0kPa的根据DIN EN ISO 3386-1:2015-10的压缩强度CLD 40%、和/或根据DIN EN ISO 8307:2008-03测量的15-60%的回弹性、和/或8至80kg/m3的泡沫密度、和/或1至250mm水柱、特别是1至50mm水柱的孔隙率。可能的生产方法描述于例如EP 2 481 770 A2或EP 2 182 020A1中。出于本发明的目的,高回弹性软质聚氨酯泡沫特别具有2.0-5.0kPa、特别是2.5-4.5kPa的根据DIN EN ISO 3386-1:2015-10的压缩强度CLD 40%、和/或根据DIN EN ISO8307:2008-03测量的≥55%的回弹性、和/或25至80kg/m3的泡沫密度、和/或1至250mm水柱、特别是1至50mm水柱的孔隙率(在压开泡沫之后)。可能的生产方法描述于例如EP1777252 B1中。出于本发明的目的,粘弹性软质聚氨酯泡沫特别具有在-20℃至+15℃范围内的玻璃化转变温度、和/或0.1-5.0kPa、特别是0.5-2.0kPa的根据DIN EN ISO 3386-1:2015-10的压缩强度CLD 40%、和/或根据DIN EN ISO 8307:2008-03测量的<10%的回弹性、和/或30至130kg/m3的泡沫密度、和/或1至250mm水柱、特别是1至50mm水柱的孔隙率(在压开泡沫之后)。可能的生产方法描述于例如WO 2013/131710 A2中。玻璃化转变温度可使用动态力学分析(DMA)(DIN 53513:1990-03)或使用差示扫描量热法(DSC)(ISO 11357-2:2013)测量。严格来说,测量的是在一定温度范围内延伸的玻璃化转变范围。
在本发明的一个优选实施方案中,本发明的床垫具有至少1cm至不大于50cm的高度和至少20cm至不大于300cm的宽度和至少20cm至不大于300cm的长度。优选的尺寸例如为5cm至40cm范围内的高度、70cm至200cm范围内的宽度、150cm至220cm范围内的长度。在本发明的一个优选实施方案中,本发明的坐垫具有至少1cm至不大于40cm的高度和至少15cm至不大于200cm的宽度和至少15cm至不大于200cm的长度。优选的尺寸例如为2cm至30cm范围内的高度、15cm至50cm范围内的宽度、15cm至50cm范围内的长度。
在本发明的又一优选实施方案中,其被配置为多区域床垫。不同的区域特别在各自的硬度方面不同。此类多区域床垫和其生产本身是已知的。它们被广泛地商业销售。特别地,所述床垫具有最多达七个不同硬度的区域,这些区域在床垫的纵向方向上延伸并且被赋予适当的宽度。当床垫具有分布于其面积上的不同硬度区域、特别是通过床垫中的切口和/或中空空间来形成时,其构成了本发明的又一优选实施方案。
在本发明的又一优选实施方案中,本发明的床垫可以是高回弹性聚氨酯泡沫床垫、粘弹性软质聚氨酯泡沫床垫、热固化的聚氨酯泡沫床垫、聚氨酯凝胶泡沫床垫、乳胶床垫或框架弹簧床垫。这些类型的床垫本身是本领域技术人员已知的,并且也以这些名称在全世界销售。为了简单起见,热固化的泡沫床垫在市场上通常被称为泡沫床垫。用于本发明目的的术语床垫还涵盖相应的床垫覆盖物和衬层。
可用于本发明上下文中的各种PUR泡沫的提供本身是已知的,并且可以求助于所有已证明的方法,条件是所述PUR泡沫是在式(I)化合物存在下生产的。相应的PUR泡沫的生产原则上不需要进一步解释,但在下文给出了用于本发明目的的PUR泡沫的生产的一些优选细节。下文将以举例方式描述本发明的主题,但本发明不限于这些说明性的实施方案。当下文详细说明化合物的范围、通式或类别时,这些意在不仅涵盖明确提到的化合物的相应的范围或类群,而且还包括可通过省去单个值(范围)或化合物而获得化合物的所有子范围和子群。当在本说明书的上下文中引用文献时,其内容、特别是关于形成其中引用所述文献的上下文的主题的内容被整体考虑,以形成本发明公开内容的一部分。除非另有说明,否则百分比是以重量百分比计的数字。当下文报告平均值时,除非另有说明,否则所讨论的值是重量平均值。当下文报告通过测量确定的参数时,除非另有说明,否则测量值已在25℃的温度和101.325Pa的压力下被确定。
出于本发明的目的,聚氨酯是由异氰酸酯、特别是多异氰酸酯和适当的异氰酸酯反应性分子获得的所有反应产物。这些包括聚异氰脲酸酯、聚脲以及含有脲基甲酸酯、缩二脲、脲二酮、脲酮亚胺或碳化二亚胺的异氰酸酯或多异氰酸酯反应产物。不言而喻,试图生产各种软质聚氨酯泡沫,例如热固化的软质聚氨酯泡沫、高回弹性软质聚氨酯泡沫或粘弹性软质聚氨酯泡沫的本领域技术人员可适当地选择在每种情况下为所述目所必需的物质,例如异氰酸酯、多元醇、稳定剂、表面活性剂等,以获得期望类型的聚氨酯,特别是期望类型的聚氨酯泡沫。所用起始材料、催化剂和助剂以及添加剂的进一步细节可见于例如Kunststoffhandbuch[Plastics Handbook],第7卷,Polyurethane[Polyurethanes],Carl-Hanser-Verlag Munich,第1版1966,第2版1983和第3版1993。下面的化合物、组分和添加剂仅作为实例被提及,可由本领域技术人员已知的其它物质替代和/或补充。
所用的异氰酸酯组分优选具有两个或更多个异氰酸酯官能团的一种或多种有机多异氰酸酯。所用的多元醇组分优选具有两个或更多个异氰酸酯反应性基团的一种或多种多元醇。
适合作为用于本发明目的的异氰酸酯组分的异氰酸酯是含有至少两个异氰酸酯基团的所有异氰酸酯。通常,可以使用本身已知的所有脂族、脂环族、芳基脂族且优选芳族多官能异氰酸酯。优选地,相对于消耗异氰酸酯的组分的总和,异氰酸酯在60mol%至350mol%范围内、更优选在60mol%至140mol%范围内使用。
具体的实例是:在亚烷基中具有4至12个碳原子的亚烷基二异氰酸酯,例如十二烷1,12-二异氰酸酯、2-乙基四亚甲基1,4-二异氰酸酯、2-甲基亚戊基1,5-二异氰酸酯、四亚甲基1,4-二异氰酸酯和优选的六亚甲基1,6-二异氰酸酯(HMDI),脂环族二异氰酸酯,如环己烷1,3-二异氰酸酯和1,4-二异氰酸酯以及这些异构体的任何期望的混合物,1-异氰酸基-3,3,5-三甲基-5-异氰酸基甲基环己烷(异佛尔酮二异氰酸酯或缩写为IPDI)、六氢亚甲苯基2,4-二异氰酸酯和六氢亚甲苯基2,6-二异氰酸酯以及相应的异构体混合物,和优选的芳族二异氰酸酯和多异氰酸酯,例如甲苯2,4-二异氰酸酯和甲苯2,6-二异氰酸酯(TDI)和相应的异构体混合物,二苯基甲烷2,4'-二异氰酸酯和二苯基甲烷2,2'-二异氰酸酯(MDI)和聚苯基聚亚甲基多异氰酸酯(粗MDI)的混合物,以及粗MDI和甲苯二异氰酸酯(TDI)的混合物。有机二异氰酸酯和多异氰酸酯可单个地使用或以其混合物的形式使用。
还可使用已通过并入氨基甲酸酯、脲二酮、异氰脲酸酯、脲基甲酸酯和其它基团而改性的异氰酸酯,其被称为改性的异氰酸酯。
因此,特别优选采用的特别适合的有机多异氰酸酯是甲苯二异氰酸酯的各种异构体(甲苯2,4-二异氰酸酯和甲苯2,6-二异氰酸酯(TDI),其呈纯形式或作为各种组分的异构体混合物)、二苯基甲烷4,4'-二异氰酸酯(MDI)、“粗MDI”或“聚合MDI”(含有MDI的4,4'异构体以及2,4'异构体和2,2'异构体和具有超过两个环的产物)以及双环产物(其被称为“纯MDI”,并且主要由2,4'异构体和4,4'异构体混合物组成)、以及由其衍生的预聚物。特别适合的异氰酸酯的实例详述在例如EP 1712578、EP 1161474、WO 00/58383、US 2007/0072951、EP 1678232和WO 2005/085310中,其以引用方式完全并入。
适合作为用于本发明目的的多元醇组分的多元醇皆为具有两个或更多个异氰酸酯反应性基团、优选OH基团的有机物质以及其配制物。优选的多元醇是通常用于生产聚氨酯体系、特别是聚氨酯泡沫的所有聚醚多元醇和/或聚酯多元醇和/或含羟基的脂族聚碳酸酯,特别是聚醚聚碳酸酯多元醇,和/或填充的多元醇(聚合物多元醇),如SAN、PHD和PIPA多元醇,其含有最高达40%或更高的固体含量的分散形式的固体有机填料;和/或自催化多元醇,其含有催化活性官能团,特别是氨基;和/或天然来源的多元醇,其被称为“基于天然油的多元醇”(NOP)。所述多元醇通常具有1.8至8的官能度和500至15 000的数均分子量。通常使用OH值在10至1200mg KOH/g范围内的多元醇。数均分子量通常通过凝胶渗透色谱(GPC),尤其是使用聚丙二醇作为参考物质和四氢呋喃(THF)作为洗脱剂来确定。OH值可特别根据DIN标准DIN 53240:1971-12来确定。取决于所得泡沫的所需的性质,可使用例如US 2007/0072951 A1、WO 2007/111828、US 2007/0238800、US 6359022或WO 96/12759中所述的适当的多元醇。其它多元醇是本领域技术人员已知的,并且可见于例如EP-A-0380993或US-A-3346557。
特别是用于生产模制且高回弹性的软质泡沫的本发明的一个优选实施方案利用了具有伯羟基、优选高于50%、更优选高于80%的双官能聚醚醇和/或三官能聚醚醇,特别是在链末端具有氧化乙烯嵌段的那些。根据依照本发明的优选的该实施方案的所需性质,尤其是对于上述泡沫的生产,优选不仅使用这里所述的聚醚醇,而且还优选使用带有伯羟基且主要基于氧化乙烯、特别是具有>70%、优选>90%的比例的氧化乙烯嵌段的其它聚醚醇。在该优选实施方案的上下文中,所述的所有聚醚醇均优选具有2至8、特别优选2至5的官能度、在2500至15 000、优选4500至12 000范围内的数均分子量和通常在5至80、优选20至50mg的KOH/g范围内的OH值。
特别是用于生产软质块料泡沫的本发明的又一优选实施方案利用了具有仲羟基、且优选高于50%、更优选高于90%的双官能聚醚醇和/或三官能聚醚醇,特别是在链末端具有氧化丙烯嵌段或无规氧化丙烯和氧化乙烯嵌段的那些,或独有地基于氧化丙烯嵌段的那些。此类聚醚醇优选具有2至8、特别优选2至4的官能度、在500-8000、优选800-5000、特别优选2500至4500范围内的数均分子量和通常在10至100、优选20至60mg的KOH/g范围内的OH值。
在本发明的又一优选实施方案中,特别是对于生产模制和高弹性的软质泡沫,使用自催化多元醇。
在本发明的又一优选实施方案中,尤其是对于生产粘弹性聚氨酯泡沫,优选使用各种、优选两种或三种多官能聚酯醇和/或聚醚醇的混合物。这里使用的多元醇组合通常由以下组成:低分子量的“交联剂”聚合物,其具有高官能度,优选具有100-270mg KOH/g的OH值;和/或常规的高分子量软质块料泡沫多元醇或HR多元醇和/或“Hypersoft”聚醚多元醇,其优选具有20至40mg KOH/g的OH值,有高比例的氧化乙烯且具有开孔的性质。
异氰酸酯和多元醇的优选比率以配方指数表示,即表示为异氰酸酯基与异氰酸酯反应性基团(例如OH基因、NH基团)的化学计量比率乘以100,该指数在10至1000、优选40至350、更优选70至140范围内。100的指数表示反应性基团摩尔比为1:1。
取决于应用,根据本发明,除了式(I)的本发明化合物之外,还可以优选使用另外的催化剂。
出于本发明的目的,表述“另外的催化剂”涵盖从现有技术已知的能够催化异氰酸酯反应和/或在多异氰酸酯反应产物、特别是聚氨酯泡沫的生产中用作催化剂、助催化剂或活化剂的所有化合物。
用于本发明目的的适合的另外的催化剂包括例如催化一种上述反应的物质,所述反应特别是胶凝反应(异氰酸酯与多元醇)、发泡反应(异氰酸酯与水)和/或异氰酸酯的二聚或三聚。此类催化剂优选含氮化合物,尤其是胺和铵盐,和/或金属化合物。
作为用于本发明目的的催化剂的适合的另外的含氮化合物的实例是胺类的三乙胺、N,N-二甲基环己胺、N,N-二环己基甲胺、N,N-二甲基氨乙基胺、N,N,N‘,N‘-四甲基亚乙基-1,2-二胺、N,N,N‘,N‘-四甲基亚丙基-1,3-二胺、N,N,N‘,N‘-四甲基-1,4-丁二胺、N,N,N‘,N‘-四甲基-1,6-己二胺、N,N,N‘,N“,N“-五甲基二亚乙基三胺、N,N,N‘-三甲基氨乙基乙醇胺、N,N-二甲氨基丙胺、N,N-二乙基氨丙基胺、1-(2-氨乙基)吡咯烷、1-(3-氨丙基)吡咯烷、N,N-二甲氨基丙基-N‘,N‘-二丙-2-醇胺、2-[[3-(二甲氨基)丙基]甲氨基]乙醇、3-(2-二甲氨基)乙氧基丙胺、N,N-双[3-(二甲氨基)丙基]胺、N,N,N‘,N“,N“-五甲基二亚丙基三胺、1-[双[3-(二甲氨基)丙基]氨基]-2-丙醇、N,N-双[3-(二甲氨基)丙基]-N',N'-二甲基丙烷-1,3-二胺、三亚乙基二胺、1,4-二氮杂二环[2.2.2]辛烷-2-甲醇、N,N‘-二甲基哌嗪、1,2-二甲基咪唑、N-(2-羟丙基)咪唑、1-异丁基-2-甲基咪唑、N-(3-氨丙基)咪唑、N-甲基咪唑、N-乙基吗啉、N-甲基吗啉、2,2,4-三甲基-2-硅杂吗啉、N-乙基-2,2-二甲基-2-硅杂吗啉、N-(2-氨乙基)吗啉、N-(2-羟乙基)吗啉、双(2-吗啉基乙基)醚、N,N’-二甲基哌嗪、N-(2-羟乙基)哌嗪、N-(2-氨乙基)哌嗪、N,N-二甲基苄胺、N,N-二甲氨基乙醇、N,N-二乙氨基乙醇、1-(2-羟乙基)吡咯烷、3-二甲氨基-1-丙醇、1-(3-羟丙基)吡咯烷、N,N-二甲基氨基乙氧基乙醇、N,N-二乙氨基乙氧基乙醇、双(2-二甲基氨乙基)醚、N,N,N'-三甲基-N'-(2-羟乙基)双(2-氨乙基)醚、N,N,N'-三甲基-N-3'-氨丙基(双氨乙基醚)、三(二甲氨基丙基)六氢-1,3,5-三嗪、1,8-二氮杂二环[5.4.0]十一-7-烯、1,5-二氮杂二环[4.3.0]壬-5-烯、1,5,7-三氮杂二环[4.4.0]癸-5-烯、N-甲基-1,5,7-三氮杂二环[4.4.0]癸-5-烯、1,4,6-三氮杂二环[3.3.0]辛-4-烯、1,1,3,3-四甲基胍、叔丁基-1,1,3,3-四甲基胍、胍、3-二甲氨基丙基脲、1,3-双[3-(二甲氨基)丙基]脲、双-N,N-(二甲氨基乙氧基乙基)异佛尔酮二氨基甲酸酯、3-二甲氨基-N,N-二甲基丙酰胺和2,4,6-三(二甲氨基甲基)苯酚。从现有技术已知的适合的另外的含氮催化剂可例如以商品名从Evonik购得。
作为另外的催化剂的适合的含金属化合物可例如选自由金属有机或有机金属化合物、金属有机或有机金属盐、有机金属盐、无机金属盐组成的组,以及选自由带电荷或不带电荷的含金属的配位化合物、特别是金属螯合物络合物组成的组。在本发明的上下文中,表述“金属有机或有机金属化合物”尤其涵盖使用具有直接碳-金属键的金属化合物,其在这里也被称为金属有机基(例如锡有机基)或有机金属化合物(例如有机锡化合物)。在本发明的上下文中,表述“有机金属盐或金属有机盐”尤其涵盖使用具有盐特性的金属有机或有机金属化合物,即其中阴离子或阳离子性质上是有机金属的离子化合物(例如有机锡氧化物、有机锡氯化物或有机锡羧酸盐)。在本发明的上下文中,表述“有机金属盐”尤其涵盖使用其中阴离子或阳离子为有机化合物的不具有任何直接碳-金属键且同时为金属盐的金属化合物(例如羧酸锡(II))。在本发明的上下文中,表述“无机金属盐”尤其涵盖使用其中阴离子和阳离子均不为有机化合物的金属化合物或金属盐,例如,金属氯化物(例如氯化锡(II))、纯金属氧化物(例如氧化锡)或混合的金属氧化物即含有多种金属,和/或金属硅酸盐或金属铝硅酸盐。在本发明的上下文中,表述“配位化合物”尤其涵盖使用由一个或多个中心粒子和一个或多个配体组成的金属化合物(例如金属-胺络合物或锡-胺络合物),其中所述中心粒子是带电荷或不带电荷的金属。出于本发明的目的,表述“金属螯合物络合物”尤其涵盖使用具有配体的含金属的配位化合物(例如金属-聚胺或锡-聚胺或金属-聚醚络合物或锡-聚醚络合物),所述配体具有至少两个与金属中心的配位或键合位置。作为用于本发明目的的另外的催化剂的尤其是如上文所定义的适合的金属化合物可例如选自所有的金属化合物,所述金属化合物含有锂、钠、钾、镁、钙、钪、钇、钛、锆、钒、铌、铬、钼、钨、锰、钴、镍、铜、锌、汞、铝、镓、铟、锗、锡、铅、和/或铋,尤其是钠、钾、镁、钙、钛、锆、钼、钨、锌、铝、锡和/或铋,更优选锡、铋、锌和/或钾。
适合的含金属的配位化合物包括例如任何金属乙酰丙酮化物,如乙酰丙酮镍(II)、乙酰丙酮锌(II)、乙酰丙酮铜(II)、二氧代乙酰丙酮钼、任何乙酰丙酮铁、任何乙酰丙酮钴、任何乙酰丙酮锆、任何乙酰丙酮钛、任何乙酰丙酮铋和任何乙酰丙酮锡。作为用于本发明目的的另外的催化剂的特别是如上文所定义的特别适合的有机金属盐和有机的金属盐,例如有机锡盐、锡盐、锌盐、铋盐和钾盐,尤其是相应的金属羧酸盐、醇盐、硫醇盐和巯基乙酸盐,例如二乙酸二丁基锡、二月桂酸二甲基锡、二月桂酸二丁基锡(DBTDL)、二月桂酸二辛基锡(DOTDL)、二新癸酸二甲基锡、二新癸酸二丁基锡、二新癸酸二辛基锡、二油酸二丁基锡、双正月桂基硫醇化二丁基锡、双正月桂基硫醇化二甲基锡、三-2-乙基己基巯基乙酸单甲基锡、双-2-乙基己基巯基乙酸二甲基锡、双-2-乙基己基巯基乙酸二丁基锡、双异辛基巯基乙酸二辛基锡、乙酸锡(II)、2-乙基己酸锡(II)(辛酸锡(II))、异壬酸锡(II)(3,5,5-三甲基己酸锡(II))、新癸酸锡(II)、蓖麻油酸锡(II)、乙酸锌(II)、2-乙基己酸锌(II)(辛酸锌(II))、异壬酸锌(II)(3,5,5-三甲基己酸锌(II))、新癸酸锌(II)、蓖麻油酸锌(II)、乙酸铋、2-乙基己酸铋、辛酸铋、异壬酸铋、新癸酸铋、甲酸钾、乙酸钾、2-乙基己酸钾(辛酸钾)、异壬酸钾、新癸酸钾和/或蓖麻油酸钾。适合的另外的金属催化剂通常且优选被选择为使得它们不具有任何引起麻烦的固有气味,并且基本上是毒理学安全的,并且使得所得聚氨酯体系、尤其是聚氨酯泡沫具有最低水平的与催化剂相关的排放。
除了另外的胺和金属化合物之外,还可使用铵盐作为另外的催化剂。适合的实例是甲酸铵和/或乙酸铵。
适合的另外的催化剂例如在DE 102007046860、EP 1985642、EP 1985644、EP1977825、US 2008/0234402、EP 0656382 B1和US 2007/0282026 A1以及其中所引用的专利文献中有提及。
所用的另外的催化剂的适合量取决于催化剂的类型,并且对于钾盐来说优选在0.01至10.0pphp(=基于100重量份多元醇的重量份)范围内,更优选在0.02至5.00pphp或0.10至10.0pphp的范围内。
式(I)的化合物可例如与适合的溶剂和/或其它添加剂一起使用。作为任选的溶剂,可使用从现有技术已知的所有适合的物质。取决于应用,可使用非质子非极性溶剂、非质子极性溶剂和质子溶剂。适合的非质子非极性溶剂可例如选自以下类别的物质或含有以下官能团的物质类别:具有低极性的芳族烃、脂族烃((烷烃(alkane,paraffin)和烯烃)、羧酸酯和聚酯、(聚)醚和/或卤代烃。适合的非质子极性溶剂可例如选自以下类别的物质或含有以下官能团的物质类别:酮、内酯、内酰胺、腈、羧酰胺、亚砜和/或砜。适合的质子溶剂可例如选自以下类别的物质或含有以下官能团的物质类别:醇、多元醇、(聚)亚烷基二醇、胺、羧酸,特别是脂肪酸和/或伯酰胺和仲酰胺。特别优选的溶剂是可在发泡操作中处理而没有任何问题且不会不利地影响泡沫性质的化合物。例如,异氰酸酯反应性化合物是适合的,因为它们通过反应被结合聚合物基质中,并且在泡沫中不会产生任何排放物。实例是OH-官能化合物如(聚)亚烷基二醇,优选单乙二醇(MEG或EG)、二甘醇(DEG)、三甘醇(TEG)、1,2-丙二醇(PG)、双丙甘醇(DPG)、三亚甲基二醇(丙烷-1,3-二醇,PDO)、四亚甲基二醇(丁二醇BDO)、丁基二甘醇(BDG)、新戊二醇、2-甲基丙烷-1,3-二醇(Ortegol CXT)和其更高级的同系物,例如具有200与3000之间的平均分子质量的聚乙二醇(PEG)。特别优选的OH-官能化合物进一步包括具有200至4500、特别是400至2000的平均分子质量的聚醚,其中优选由水-、烯丙基-、丁基-或壬基-引发的聚醚,特别是基于氧化丙烯(PO)和/或氧化乙烯(EO)嵌段的那些。
当以溶解的形式或与溶剂组合来使用式(I)的化合物,或使用式(I)化合物与另外的催化剂的预混合催化剂组合时,所有催化剂的总和与溶剂的质量比率优选在100:1至1:4、优选50:1至1:3、更优选25:1至1:2范围内。
所用的任选的添加剂可以是根据现有技术已知且可用于生产聚氨酯、特别是聚氨酯泡沫的所有物质,例如用于形成CO2的发泡剂、优选水,以及如果需要,其它物理发泡剂、交联剂和扩链剂、抗氧化降解的稳定剂(称为抗氧化剂)、阻燃剂、表面活性剂、杀生物剂、泡孔改进添加剂、开孔剂、固体填料、抗静电添加剂、成核剂、稠化剂、染料、颜料、色浆、香料、乳化剂、缓冲物质和/或另外的催化活性物质,尤其是如上文所定义的。
水通常在软质聚氨酯泡沫的生产中用作发泡剂。优选使用如下量的水,所述量使得水的浓度为0.10至25.0pphp(pphp=基于100重量份多元醇的重量份)。
还可使用适合的物理发泡剂。这些是例如液化的CO2和挥发性液体,例如具有3个、4个或5个碳原子的烃,优选环戊烷、异戊烷和正戊烷,含氧化合物,如甲酸甲酯、丙酮和二甲氧基甲烷,或氯化烃,优选二氯甲烷和1,2-二氯乙烷。
除了水和物理发泡剂以外,还可使用与异氰酸酯反应而放出气体的其它化学发泡剂,例如甲酸。
任选的交联剂和任选的扩链剂是对异氰酸酯具有反应性的低分子量的多官能化合物。适合的化合物是例如羟基或胺封端的物质,如甘油、新戊二醇、2-甲基-1,3-丙二醇、三乙醇胺(TEOA)、二乙醇胺(DEOA)和三羟甲基丙烷。使用浓度通常基于100份多元醇在0.1-5份的范围内,但也可取决于配制物而偏离该范围。当粗MDI被用于原位发泡时,其同样具有发挥交联功能。因此,低分子量交联剂的含量可随着粗MDI的量的增加而相应地降低。
抗氧化降解的适合的任选稳定剂被称为抗氧化剂,其优选所有标准的自由基清除剂、过氧化物清除剂、UV吸收剂、光稳定剂、用于金属离子污染物的络合剂(金属钝化剂)。优选使用以下类别的物质或含有以下官能团的物质类别的化合物,其中各自的母体分子上的取代基优选特别是具有对异氰酸酯有反应性的基团的取代基:2-(2'-羟苯基)苯并三唑、2-羟基二苯甲酮、苯甲酸和苯甲酸酯、酚类,特别是在芳族实体上包含叔丁基和/或甲基取代基的酚类、苯并呋喃酮、二芳基胺、三嗪、2,2,6,6-四甲基哌啶、羟胺、亚磷酸烷基酯和亚磷酸芳基酯、硫化物、羧酸锌、二酮。
在本发明的上下文中,适合的任选阻燃剂是根据现有技术被认为适合于该目的的所有物质。优选的阻燃剂是例如液体有机磷化合物,如不含卤素的有机磷酸酯,例如磷酸三乙酯(TEP),卤代磷酸酯,例如磷酸三(1-氯-2-丙基)酯(TCPP)和磷酸三(2-氯乙基)酯(TCEP),和有机膦酸酯,例如甲烷膦酸二甲酯(DMMP)、丙烷膦酸二甲酯(DMPP),或固体,如聚磷酸铵(APP)和红磷。适合的阻燃剂还包括卤代化合物,例如卤代的多元醇,以及固体,如可膨胀石墨和三聚氰胺。
聚氨酯泡沫的泡沫性质可任选地在其生产过程中使用特别是硅氧烷或有机改性的硅氧烷来影响,对此可以使用现有技术中已知的物质。优选使用特别适于各自泡沫类型(硬质泡沫、热固化软质泡沫、粘弹性泡沫、酯泡沫、高回弹性软质泡沫(HR泡沫)、半硬质泡沫)的化合物。适合的(有机改性的)硅氧烷描述于例如以下文献中:EP 0839852、EP1544235、DE 102004001408、EP 0839852、WO 2005/118668、US 20070072951、DE 2533074、EP 1537159、EP 533202、US 3933695、EP 0780414、DE 4239054、DE 4229402、EP 867465。这些化合物可如现有技术中所述来制备。适合的实例描述于例如US 4147847、EP 0493836和US 4855379中。
作为任选的(泡沫)稳定剂,可使用从现有技术已知的所有稳定剂。优选使用如通常用于生产氨基甲酸酯泡沫的基于聚二烷基硅氧烷-聚氧化烯共聚物的泡沫稳定剂。这些化合物的结构优选使得例如氧化乙烯和氧化丙烯的长链共聚物键合至聚二甲基硅氧烷基。聚二烷基硅氧烷和聚醚部分之间的键接可通过SiC键接或Si-O-C键实现。在结构方面,聚醚或不同的聚醚可于末端或侧向位置键合至聚二烷基硅氧烷。烷基或各种烷基在这里可以是脂族、脂环族或芳族的。甲基是非常特别有利的。聚二烷基硅氧烷可以是直链的,或含有支链。适合的稳定剂、尤其是泡沫稳定剂尤其描述于US 2834748、US2917480以及US 3629308中。适合的稳定剂可以商品名购自Evonik Industries AG。
在本发明的上下文中(尤其是在本发明应用的上下文中),硅氧烷也可用作具有不同载体介质的组合物的一部分。有用的载体介质包括例如二醇,例如单乙二醇(MEG)、二甘醇(DEG)、丙二醇(PG)或双丙甘醇(DPG)、烷氧基化物或合成和/或天然来源的油。
可优选以如下量将所述硅氧烷添加到用于生产聚氨酯泡沫的组合物中,所述量使得成品聚氨酯泡沫中的硅氧烷的质量比为0.01重量%至10重量%、优选0.1重量%至3重量%。
在软质聚氨酯泡沫的生产中可能有利的是,生产和/或使用包含至少一种式(I)的本发明化合物、至少一种多元醇组分、任选存在的至少一种异氰酸酯组分和任选存在的一种或多种发泡剂的组合物并使该组合物反应。特别优选使用包含上文已描述用于生产软质聚氨酯泡沫、特别是这种类型的热固化泡沫、高回弹性泡沫和粘弹性泡沫的材料或组分的组合物。
出于本发明的目的,式(I)的本发明化合物明确涵盖相应的季铵化化合物和/或质子化化合物。然而,根据本发明,特别优选使用未季铵化或未质子化的式(I)化合物。对于式(I)化合物的可能的季铵化,可使用称为季铵化试剂的任何试剂。优选使用烷基化试剂,如硫酸二甲酯、氯甲烷或苄基氯,优选甲基化试剂作为季铵化试剂,如特别是硫酸二甲酯。同样可使用氧化烯如氧化乙烯、氧化丙烯或氧化丁烯实施季铵化,优选随后使用无机酸或有机酸中和。式(I)的化合物如果被季铵化,则可被单一或多重季铵化。优选地,式(I)的化合物仅被单一季铵化。在单一季铵化的情况下,式(I)的化合物优选在作为环、优选吡咯烷环的一部分的氮原子上被季铵化。式(I)的化合物可通过与有机酸或无机酸反应而转化成相应的质子化化合物。例如当要实现例如减慢的聚氨酯反应时,或当反应混合物要在使用中具有增强的流动行为时,可优选这些质子化化合物。作为有机酸,可使用例如下文所述的所有有机酸,例如具有1至36个碳原子的羧酸(芳族或脂族、直链或支链),例如甲酸、乳酸、2-乙基己酸、水杨酸和新癸酸,或聚合酸,如聚丙烯酸或聚甲基丙烯酸。作为无机酸,可使用例如基于磷的酸、基于硫的酸或基于硼的酸。
包含式(I)化合物以及另外的胺催化剂的含氮催化剂的总量与多元醇组分的异氰酸酯反应性基团的总量的摩尔比优选4×10-4:1至0.2:1。
式(I)的含氮化合物优选以对应于以下质量比例的总量使用:基于100份(pphp)多元醇组分0.01至20.0份(pphp)、优选0.01至5.00份且特别优选0.02至3.00份。
根据本发明的聚氨酯泡沫的生产可通过本领域技术人员熟悉的所有方法实施,例如以手动混合工艺或优选借助发泡机、特别是低压或高压发泡机实施。这里可使用间歇处理器或连续处理器。
可使用本领域技术人员已知的用于生产聚氨酯泡沫的所有工艺。例如,发泡操作可在水平或垂直方向上,在间歇式设备或连续设备中进行。根据本发明所用的组合物类似地可用于CO2技术。用于低压机和高压机中是可能的,其中能够将待处理的组合物直接计量加入混合室中,或甚至在混合室之前与随后进入混合室的一种组分混合。在原材料罐中混合也是可以的。
用于本发明目的的非常特别优选的软质聚氨酯泡沫特别具有以下组成:
本发明进一步提供软质聚氨酯泡沫在床垫和/或坐垫、特别是床垫中的用途,其中所述软质聚氨酯泡沫已通过在式(I)化合物存在下使至少一种多元醇组分和至少一种异氰酸酯组分反应而获得:
在这方面,可特别参考上文所述的内容,其也适用于本主题。
根据本发明的用途使得可提供具有改进的抗老化性和改进的排放行为的床垫和/或坐垫。
具体实施方式
实施例
软质聚氨酯泡沫的物理性质:
借助以下物理性质来评估所生产的软质聚氨酯泡沫:
a)上升阶段结束后的泡沫回落(=沉降):从直接吹离后的泡沫高度和泡沫吹离后3分钟后的泡沫高度的差异找出泡沫的沉降或进一步上升。泡沫高度是借助于固定至厘米标尺(centimetre scale)的针在泡沫顶部的中间以最大值测量的。这里的负值描述了泡沫在吹离后的沉降;正值相应地描述了泡沫的进一步上升。
b)泡沫高度:泡沫的最终高度通过从吹离后的泡沫高度减去沉降或将进一步上升加到吹离后的泡沫高度来确定。以厘米(cm)报告泡沫高度。
c)泡沫密度(FD):如ASTM D 3574-11(测试A)中所述通过测量核心密度来进行泡沫密度的确定。以kg/m3报告泡沫密度。
d)孔隙率:通过对泡沫的动态压力测量来确定泡沫的透气率。以mm水柱报告测量的动态压力,较低的动态压力值表征更开放的泡沫。测量的值在0至300mm的范围内。
借助包括氮源、具有压力计的减压阀、流量调节旋钮、洗瓶、流量计、T形件、施加器喷嘴和填充有水的有刻度的玻璃管的装置测量动态压力。施加器喷嘴具有100×100mm的边缘长度、800g的重量、5mm的出口开口内径、20mm的下施加环内径和30mm的下施加环外径。
通过借助于减压阀将氮气进入压力设定为1巴并将流动速率设定为480l/h来实施测量。设定有刻度的玻璃管中的水量,使得不会积累压力差并且不能读出。对于具有250×250×50mm的尺寸的测试样本的测量,将施加器喷嘴放置到测试样本的角上,与边缘齐平,并且还在测试样本的(估计的)中心上放置一次(每种情况下都是在具有最大表面积的一侧)。当已建立恒定的动态压力时,读出结果。
通过形成所获得的五次测量的平均值进行评价。
e)根据DIN EN ISO 3386-1:2015-10的压缩强度CLD 40%。以千帕斯卡(kPa)报告测量值。
通过测试室测试(PC)确定室温排放:
在室温下通过基于DIN方法DIN EN ISO 16000-9:2008-04的程序确定所得泡沫的排放、特别是与催化相关的排放或它们的分解或反应产物。在24小时后进行取样。为此,将2升测试室气氛以100ml/min的流动速率通过填充有Tenax TA(35/60目)的吸附管。下文描述了用随后连接的气相色谱/质谱(GC-MS)实施热解吸的程序。
a)测量技术:使用具有来自Gerstel,Mülheim的自动取样器的"TDS2"热解析器,结合Agilent 7890/5975GC/MSD系统实施热解吸。
b)测量条件示于表1和表2中。
表1:用于测试室测量的热解吸测量参数。
表2:用于测试室测量的气相色谱/质谱测量参数。
c)为了校准,将甲苯和十六烷(各自为0.125mg/ml)在甲醇中的2μl混合物置于填充有TA(35/60目)的清洁吸附管中,并进行测量(解吸5min;280℃)。
软质泡沫-发泡实施例
实施例1:软质聚氨酯泡沫(软质块料泡沫)的生产
使用表3中所示的泡沫配制物来实施式(I)化合物的性能测试。
表3:用于软质块料泡沫应用的配制物1。
1)具多元醇1:具有48mg KOH/g的OH值的基于甘油的聚醚多元醇。
2)可从Evonik Industries获得的29:2-乙基己酸的锡(II)盐。
3)聚醚改性的聚硅氧烷。
4)T 80甲苯二异氰酸酯(80%的2,4-异构体、20%的2,6-异构体),来自Bayer,3mPa·s,48%的NCO,官能度为2。
在发泡操作中,使用了500g多元醇;相应地调节其它配制物组分。这里,例如,1.00份组分意指每100g多元醇的1.00g物质。
通过手动混合来产生泡沫。使用各种胺催化剂,采用如表3中所示的配制物1。为此,将多元醇、常规或本发明的含氮催化剂(胺)、锡催化剂、水和泡沫稳定剂称入杯中并在1000rpm下混合60秒。在添加异氰酸酯(TDI)后,将反应混合物在2500rpm下搅拌7s,并立即转移至纸内衬的箱子(27cm×27cm基底面积和27cm高度)中。为了评估催化性质,确定以下特征参数:上升时间、上升高度和上升阶段结束后的泡沫回落(=沉降):
从得到的泡沫块上切下所限定的泡沫体,并进一步分析。对样本确定以下物理性质:泡沫密度(FD)、孔隙率(=空气渗透率)和压缩强度CLD(40%)。
式(I)的本发明的含氮化合物的催化性质以及所得软质块料泡沫的物理性质的评价结果汇总于表4中。作为根据现有技术的比较催化剂,使用三亚乙基二胺于双丙甘醇中的33重量%浓度的溶液(33,可从Evonik Industries获得)、2-[2-(二甲基氨基)乙氧基]乙醇(DMEE,可从Evonik Industries获得)和双(2-二甲基氨乙基)醚于双丙甘醇中的70重量%浓度的溶液(BDE,可从Evonik Industries获得)。在每种情况下使用0.20pphp(=基于100重量份多元醇的重量份)的胺。
表4:配制物1(表3)的发泡结果。
1)=(动态压力,mm水柱)。
从表4中可以看出,式(I)的本发明化合物展示出在发泡反应方面的高催化活性和选择性,这与未经平衡的33的相比是明显的。在发泡反应方面的催化的高选择活性与BDE的选择活性几乎相当,并且大大优于DMEE的选择活性。所得泡沫的物理评价还显示,例如在开孔比例方面,式(I)的化合物是高选择性和高活性的发泡催化剂。
实施例2:来自软质块料聚氨酯泡沫的排放
为了研究式(I)的化合物对泡沫排放的影响,使用表5中所示的泡沫配制物,其含有低排放多元醇和低排放锡催化剂。
表5:软质块料泡沫应用中的配制物2泡沫排放。
1)多元醇1:具有56mg KOH/g的OH值的低排放的基于甘油的聚醚多元醇。
2) EF,可自Evonik Industries获得:蓖麻油酸的锡(II)盐。
3)聚醚改性的聚硅氧烷。
4)T 80甲苯二异氰酸酯(80%的2,4-异构体、20%的2,6-异构体),来自Bayer,3mPa·s,48%的NCO,官能度为2。
在发泡操作中,使用了500g多元醇;相应地调节其它配制物组分。这里,例如,1.00份组分意指每100g多元醇的1.00g物质。
通过手动混合来实施发泡。使用如表5中所详细说明的含有各种胺催化剂的配制物2。为此,将低排放多元醇、常规或本发明的含氮催化剂(胺)、低排放锡催化剂、水和泡沫稳定剂称入杯中,并在1000rpm下混合60秒。在添加异氰酸酯(TDI)后,将反应混合物在2500rpm下搅拌7s,并立即转移至纸内衬的箱子(27cm×27cm基底面积和27cm高度)中,并且在所得泡沫吹离后,以气密方式将其密封在聚乙烯膜中。在24小时的固化阶段之后,从所得泡沫块中切出限定的泡沫立方体(7cm×7cm×7cm),将其完全包封在铝箔中,并另外借助于聚乙烯膜密封。
随后通过基于如上所述的DIN方法DIN EN ISO 16000-9:2008-04的测试室测试,在室温下检查上述泡沫的排放特征。结果示于表6中。
表6:来自配制物2(表5)的软质块料泡沫的排放
通过测试室测试对挥发性有机化合物的含量的确定
1)TC总=总排放;TC胺=测试室测试中所有挥发性胺或胺组分的排放。
表6显示,与非反应性胺如BDE或33相比,当使用式(I)的化合物时,可令人惊讶地降低胺排放,并且与可并入的VOC优化胺如DMEE一样获得类似的值。因此特别是与使用BDE相比,可通过替代使用式(I)的化合物来生产具有显著降低的胺排放的软质聚氨酯块料泡沫;在这种情况下,甚至可获得不含或几乎不含胺排放物的泡沫。另外,从表4(实施例1)可以看出,当使用式(I)的化合物时,与反应性胺如DMEE相比,可显著缩短上升时间,其组合表示在用于生产软质块料泡沫中有相当大的优点。因此,式(I)的化合物表示高活性、发泡选择性和低排放的胺催化剂。
实施例3:软质聚氨酯块料泡沫的老化
用于根据DIN标准DIN EN ISO 2440/A1:2009-01进行老化测试的软质块料泡沫是借助于配制物1(表3)以类似于实施例1的方式生产的。选择在140℃(烘箱)下进行2小时的干热老化作为老化方法。将适于计算根据DIN EN ISO 3386-1:2015-10的压缩强度CLD40%的泡沫立方体(10cm×10cm×5cm)充当测试样本。首先,为了比较的目的,对来自相同泡沫块的适合的测试样本确定老化前的压缩强度。在可能时,同样确定老化过的测试样本的压缩强度。使用低排放胺催化剂2-[2-(二甲基氨基)乙氧基]乙醇(DMEE,可从Evonik Industries获得)作为根据现有技术的比较催化剂。结果编制于表7中。
表7:软质块料泡沫在干热老化之前和之后的压缩强度的变化。
从表7可以看出,不管所选的胺催化剂如何,两个测试样本在干热老化之前具有相当的压缩强度。当使用式(I)的化合物时,在热老化之后也没有观察到压缩强度的显著退化。这是出人意料的,因为低排放的催化剂通常会导致泡沫老化性质受损。这也通过低排放催化剂DMEE的实例显示,其中测量到老化后压缩强度的显著降低。在DMEE的情况下,选择的热老化甚至导致泡沫结构的相当大的破坏。当使用式(I)的化合物时,则没有观察到这种情况。因此,式(I)的化合物代表了用于生产高活性、非常高的发泡选择性、低排放的抗老化软质聚氨酯泡沫的胺催化剂。
本发明的有利性质也在其它类型的泡沫(例如高回弹性软质泡沫(块料泡沫和模制泡沫))的情况下得到证实。
式(I)的本发明化合物的制备
合成实施例1:
将26.74g(0.187mol)2-氯乙基醚置于装配有搅拌器、可加热夹套、压力计和温度传感器以及惰性气体入口管线的250ml实验用高压釜中,并与120.0g(1.68mol)量的吡咯烷混合。在借助于氮气使实验用高压釜惰性化后,将高压釜加热至60℃的夹套温度并保持12小时,未能观察到显著的压力上升。出于去活性的目的,然后施加20毫巴的减压以去除未反应的初始材料。然后用氮气冲洗该实验用高压釜,并将反应残余物在隔膜泵真空中进行精馏。在大量未反应的吡咯烷酮在所述工艺过程中经过之后,在15毫巴和161℃的顶部温度下,可驱使对应于56%收率的量的22.23g产物在目标馏分中经过。含有大量季铵化副产物的反应底部产物在冷却时结晶,得到棕色的盐样物质。对目标馏分的13C-NMR以及GC-MS分析对应于预期,并确认了产物的形成。
Claims (13)
1.包含至少一个区段的软质聚氨酯泡沫的床垫和/或坐垫,其特征在于所述软质聚氨酯泡沫已通过在式(I)化合物和至少一种发泡剂存在下使至少一种多元醇组分和至少一种异氰酸酯组分反应而获得:
2.根据权利要求1所述的床垫和/或坐垫,其特征在于所述软质聚氨酯泡沫是热固化的软质聚氨酯泡沫、高回弹性软质聚氨酯泡沫或粘弹性软质聚氨酯泡沫,或者特征在于使用这些软质泡沫的组合。
3.根据权利要求1或2所述的床垫和/或坐垫,其特征在于所述软质聚氨酯泡沫具有根据DIN EN ISO 8307:2008-03测量的1-80%的回弹性、和/或5至150kg/m3的泡沫密度、和/或1至250mm、特别是1至50mm水柱的任选地在压开所述泡沫之后的孔隙率。
4.根据权利要求1至3中任一项所述的床垫和/或坐垫,其特征在于所述软质聚氨酯泡沫具有0.1至8.0kPa的根据DIN EN ISO 3386-1:2015-10的压缩强度CLD 40%。
5.根据权利要求1至4中任一项所述的床垫和/或坐垫,其特征在于所述软质聚氨酯泡沫是热固化的软质聚氨酯泡沫,并且优选具有2.0-8.0kPa的根据DIN EN ISO 3386-1:2015-10的压缩强度CLD 40%、和/或根据DIN EN ISO 8307:2008-03测量的15-60%的回弹性、和/或8至80kg/m3的泡沫密度、和/或1至250mm、特别是1至50mm水柱的孔隙率。
6.根据权利要求1至4中任一项所述的床垫和/或坐垫,其特征在于所述软质聚氨酯泡沫是高回弹性软质聚氨酯泡沫,并且优选具有2.0-5.0kPa、特别是2.5-4.5kPa的根据DINEN ISO 3386-1:2015-10的压缩强度CLD40%、和/或根据DIN EN ISO 8307:2008-03测量的≥55%的回弹性、和/或25至80kg/m3的泡沫密度、和/或1至250mm、特别是1至50mm水柱的优选在压开所述泡沫之后的孔隙率。
7.根据权利要求1至4中任一项所述的床垫和/或坐垫,其特征在于所述软质聚氨酯泡沫是粘弹性软质聚氨酯泡沫,并且优选具有在-20℃至+15℃范围内的玻璃化转变温度、和/或0.1-5.0kPa、特别是0.5-2.0kPa的根据DIN EN ISO 3386-1:2015-10的压缩强度CLD40%、和/或根据DIN EN ISO 8307:2008-03测量的<10%的回弹性、和/或30至130kg/m3的泡沫密度、和/或1至250mm、特别是1至50mm水柱的优选在压开所述泡沫之后的孔隙率。
8.根据权利要求1至7中任一项所述的床垫,其特征在于其具有至少1cm至不大于50cm的高度和至少20cm至不大于300cm、优选至少70cm至不大于200cm的宽度,以及至少20cm至不大于300cm、优选至少150cm至不大于220cm的长度。
9.根据权利要求1至8中任一项所述的床垫,其特征在于其被配置为多区域床垫。
10.根据权利要求1至9中任一项所述的床垫,其特征在于其具有分布于其面积上的不同硬度区域,所述不同硬度区域特别通过在所述床垫中的切口和/或中空空间来形成。
11.根据前述权利要求中任一项所述的床垫,其中所述床垫是高回弹性泡沫床垫、粘弹性床垫、凝胶泡沫床垫、乳胶床垫或框架弹簧床垫。
12.软质聚氨酯泡沫在床垫和/或坐垫、特别是床垫中的用途,其中所述软质聚氨酯泡沫已通过在式(I)化合物存在下使至少一种多元醇组分和至少一种异氰酸酯组分反应而获得:
13.根据权利要求12所述的用途,其用于提供具有改进的抗老化性和改进的排放行为的床垫和/或坐垫。
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