CN113993678A - 聚氨酯泡沫层的高生产量制造 - Google Patents
聚氨酯泡沫层的高生产量制造 Download PDFInfo
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- CN113993678A CN113993678A CN202080045396.5A CN202080045396A CN113993678A CN 113993678 A CN113993678 A CN 113993678A CN 202080045396 A CN202080045396 A CN 202080045396A CN 113993678 A CN113993678 A CN 113993678A
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- foam
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- polyurethane
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Images
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Abstract
本发明涉及一种至少部分连续的工艺,其用于以比本领域通常可实现的更高生产量制造适用于医疗应用(尤其是伤口敷料)的聚氨酯泡沫层。所述工艺包括PU泡沫的加速固化步骤,该步骤在整个固化过程的阶段进行,在该阶段,失控反应的风险被最小化。
Description
技术领域
本发明涉及一种用于制造聚氨酯泡沫层的至少部分连续的高生产量工艺,所述聚氨酯泡沫层适用于医疗应用,特别是伤口敷料。所述工艺包括PU泡沫的加速固化步骤,该步骤在整个固化过程的阶段进行,在该阶段,失控反应的风险被最小化。
背景技术
伤口敷料用于愈合和保护伤口。伤口敷料的吸收和保留伤口渗出物的能力对于愈合过程至关重要。敷料的液体处理能力也影响敷料更换的频率,为了促进伤口愈合,应最小化更换频率。特别地,亲水性材料用于伤口敷料中以吸收和保留伤口流体,进一步特别是亲水性泡沫,比如亲水性开放孔聚氨酯(PU)泡沫。
制造特别适用于医疗应用的PU泡沫的工艺从现有技术中已知,例如从US 5 254301中已知,该专利公开了一种制造聚合物基泡沫板,特别是异氰酸酯封端的聚醚基泡沫的连续工艺。该工艺特别在室温下进行,并且通过在固化过程中应用的泡沫压缩步骤来调节层的厚度。该工艺在室温下进行的事实意味着用于进一步激活固化过程的热量仅源于放热反应。在室温下进行PU泡沫,尤其是TDI-基泡沫的固化,并且不通过从外部增加温度来增加固化速率,是因为这些泡沫的固化/交联反应很容易被加速到无法控制。
US 2019/0083675描述了另一种制造亲水性泡沫的工艺,该专利公开了制造包含聚氨酯泡沫基质的多层泡沫的工艺。将反应性预聚物混合物沉积在(第一)泡沫层基底上,并使反应产物升高。为了调节所需的最终厚度,在固化步骤期间泡沫层被压缩。
现有技术中已知的制造PU泡沫的工艺通常需要全批量处理(参见例如US 2015/0011666)和/或相对大的生产线和/或与相对低的线速度相关联。相对低的线速度通常被认为是必需的,特别是对于反应性预聚物混合物(比如包含TDI的混合物),因为较低的线速度增加了生产线中给定泡沫段的停留时间(例如在干燥和/或储存之前),因此允许泡沫层完全(或至少充分)固化。
发明内容
基于如上所述的现有技术和背景,本领域需要提供制造聚氨酯泡沫的工艺,该工艺允许在比在本领域已知的工艺中通常可实现的更短的时间间隔内更高的泡沫生产量,特别是用于适合医疗应用的泡沫的生产,。这种工艺应该避免或最小化本领域工艺已知的至少一个缺点,并且应该允许改进的工艺控制,特别是避免或最小化“失控”固化/交联反应,同时仍然允许高生产量处理。
根据本发明的第一方面,通过制造聚氨酯泡沫层的工艺实现这些和其他目的,其中所述工艺至少包括以下步骤:
(i)至少一个混合步骤,其中一种或更多种聚氨酯预聚物或其前体在混合区域或接触区域中相互混合或接触,和/或与另一种组分混合或接触;
(ii)至少一个层形成步骤,其中来自步骤(i)的混合物以形成层的方式施加到移动的基底上,并在基底上开始固化过程;
(iii)至少一个输送步骤,在该步骤中,来自步骤(ii)的基底上的泡沫层沿着生产线至少部分地移动,在该步骤中,泡沫层中的聚氨酯预聚物或其前体至少部分地固化,并且由于发泡,即由于在该层中发生的至少一个化学反应,该层的厚度增加;
(iv)至少一个加速固化的步骤,其发生在步骤(ii)结束后的时间预定点,或者相应地,发生在沿着生产线的预定位置,其中通过使在基底上移动的泡沫经受辐射加热,优选经受红外辐射来加速固化。
在本发明的实施方案中,该工艺包括以下附加步骤,其在步骤(iv)之后实施:
(v)与步骤(iv)分开并在其结束后:至少一个干燥步骤,在此期间,将来自步骤(iv)的基本固化的湿泡沫干燥以达到预定的较低含水量。
在优选实施方案中,基本上固化的湿泡沫包含至少10%w/w的水、优选至少30%w/w的水、进一步优选至少50%w/w的水,并且干燥以达到等于或小于10%w/w、优选小于5%w/w、进一步优选小于2%w/w的预定含水量。
步骤(i)的预聚物
在混合或接触步骤(i)中,一种或更多种预聚物或其前体可以与自身或与其它组分混合。其他组分尤其可以是溶剂,尤其是质子溶剂,进一步尤其是水。其他组分也可以是或另外是另一种前体或聚合物。
还包括两种或更多种组分的混合,特别是组成预聚物的前体或在所谓的“一步法”中快速混合在一起的前体。
在本发明的实施方案中,混合或接触步骤(i)是或包括将至少一种预聚物与水混合的步骤。
对于预聚物、前体或添加的任何其它组分,或对于步骤(i)中使用的全部混合物不存在限制,只要该混合物产生适用于医疗敷料的聚氨酯泡沫。
根据本发明,术语“预聚物”应理解为在lUPAC中定义的:Compendium of ChemicalTerminology,第二版。(“Gold Book”),由A.D.McNaught和A.Wilkinson编纂。BlackwellScientific Publications,Oxford(1997),ISBN 0-9678550-9-8,通常指的是其分子能够通过反应性基团进入进一步聚合,从而为最终聚合物的至少一种类型的链贡献一个以上结构单元的聚合物或低聚物。
在本发明的实施方案中,预聚物可以包含或为异氰酸酯封端的多元醇或异氰酸酯封端的聚氨酯。
在本发明的实施方案中,预聚物来源于多元醇和二异氰酸酯化合物之间的反应,其中所述二异氰酸酯化合物选自六亚甲基二异氰酸酯(HDI)、甲苯二异氰酸酯(TDI)、亚甲基二苯基二异氰酸酯(MDI)或异佛尔酮二异氰酸酯(IPDI)或其任意混合物。
甲苯二异氰酸酯(TDI)或包含TDI的混合物通常优选用于医疗敷料,因为它们作为亲水性聚氨酯泡沫的性能得到改善。
步骤(i)的混合物的其它化合物:
对于步骤(i)的预聚物或前体混合物中其它化合物或组分的存在没有限制,只要这些其它化合物或组分不会使所得PU泡沫不适合医疗应用,特别是伤口护理应用。
包括在步骤(i)的混合物中的合适组分例如是水(用作溶剂和/或“化学”发泡剂)、表面活性剂(湿润剂)、催化剂、溶剂(除水之外的溶剂)、发泡剂、增链剂、亲水剂、交联剂、颜料、填料颗粒、助剂、附加的聚合物组分等..
在本发明的实施方案中,混合物进一步包含至少一种表面活性剂,优选非离子表面活性剂。
步骤(ii):“基底”和固化的开始
固化给定预聚物或前体混合物,例如通过多元醇的OH-基团和多异氰酸酯的异氰酸酯基团之间的化学反应,或通过水和异氰酸酯基团之间的化学反应(例如,在制造包含预聚物的水性混合物的步骤中,该步骤包括将包含预聚物的预聚物组合物与水混合的步骤)通常将从至少两种组分混合物彼此接触的时刻开始,即已经在步骤(i)中,或甚至更早。然而,为了根据本发明的固化工艺的定时,固化工艺的“开始”被定义为在步骤(ii)中将来自步骤(i)的预聚物或前体混合物的给定体积段施加到移动基底上的时刻。
根据本发明使用的术语“固化”特别包括混合物中预聚物的聚合物之间的键的形成,特别地交联键是或包括通过第一聚合物上的羟基和第二聚合物上的异氰酸酯(NCO)基团之间的反应形成的氨基甲酸酯键,或通过第一聚合物上的胺基和第二聚合物上的异氰酸酯(NCO)基团之间的反应形成的脲键。
根据本发明,术语“固化”包括“交联”,即交联是一个方面,优选是整个固化工艺的主要效果。
术语“交联”在本文中用于描述包含多个聚合物分子的材料,这些聚合物分子通过化学键,特别是共价键或离子键,或通过物理交联相互连接。
在本发明的实施方案中,将来自步骤(i)的预聚物或前体以混合或聚集在一起的方式施加到移动的基底上,从而在基底上产生给定的“涂层重量”(“涂层重量”=每平方厘米基底分配的混合物的克数)。所述涂层重量适于产生所需的最终泡沫层厚度。在本发明的实施方案中,所述克重为30g/m2至1000g/m2,优选50g/m2至500g/m2,进一步优选75g/m2至250g/m2。这些克重通常对应于可被辐射,特别是IR辐射适当穿透的薄膜厚度,如步骤(iv)中所用。
根据本发明使用的“层”应该理解为在一个平面(x和y方向)上具有连续的延伸,并且厚度垂直于所述平面(z方向)。根据本发明,最终产生的泡沫层的长度(通常为准备储存的干燥和固化层的卷起批次)比该层的宽度大至少一个数量级。该层的宽度比该层的厚度大至少5倍。
对于所述移动基底的具体实现不应用限制,只要所述基底能够容纳来自步骤(i)的预聚物或前体混合物而基本上不与其反应(即相对于预聚物/前体混合物基本上是惰性的),并且能够在预聚物混合物固化时沿着整个生产线的至少一部分输送给定体积段的预聚物混合物(即,至少在一个方向上将其转移),并且最终允许移除(基本上)固化的聚氨酯泡沫或固化并干燥的聚氨酯泡沫。
在本发明的实施方案中,基底被实现为移动输送带,优选地被实现为移动纤维网(web)。
在本发明的其他实施方案实施方案中,基底被实现为移动的释放衬垫,该衬垫随后被移除(“牺牲层”)。合适的材料是涂覆硅酮的或涂覆含氟聚合物的释放衬垫。涂覆硅酮的衬垫是优选的。
此外,对于如何将步骤(i)的混合物施加到基底上没有限制。优选地通过喷嘴施加。更优选地,喷嘴被设置为狭缝,该狭缝限定了存在于基底上的层的初始宽度和初始厚度。
在本发明的实施方案中,施加在基底上的泡沫层,即在步骤(ii)开始时的泡沫层的初始厚度为100μm至8mm,优选为250μm至2mm。
输送步骤(iii)
在本发明的实施方案实施方案中,在所述输送步骤(iii)中,泡沫的给定体积段被线性输送至少3m,优选不小于10m,进一步优选不小于20m。进一步优选的范围是20m至80m或30m至50m。
在本发明的实施方案实施方案中,在所述输送步骤(iii)中,泡沫的给定体积段被输送36秒至900秒,优选为180秒至320秒。
加速固化步骤(iv)
在本发明的实施方案中,步骤(iv)的时间“预定点”可以由层的厚度、固化度或任何其他合适的参数,特别是温度来确定,在该时间点,所输送的泡沫层的给定体积段经受辐射加热。测量这些预定点中任何一个的参考点是步骤(ii)的开始,即沿生产线的时间点,在该时间点处,来自步骤(i)的预聚物或前体混合或聚集在一起并施加到移动的基底上。
在本发明的实施方案中,当泡沫的厚度相对于最初在步骤(ii)中施加的层的厚度增加至少60%,优选至少80%时,达到步骤(iv)中的所述时间“预定点”。
在本发明的实施方案中,当已经达到泡沫固化的峰值温度时,优选地当峰值温度已经过去时,即温度已经从最大值下降或开始下降时,达到步骤(iv)中的所述时间“预定点”。
根据本发明,“峰值温度”是在步骤(iii)的预定点在泡沫的表面测量的最高或最大温度。所述温度适合用红外温度传感器测量。
在本发明的实施方案中,在步骤(iii)开始时温度在18℃至24℃,优选地18℃至23℃的范围内之后,当泡沫层的温度在25℃至35℃,优选地27℃至32℃的范围内时,达到步骤(iv)中的所述时间“预定点”。
在本发明的实施方案中,在步骤(iii)开始后2至10分钟,优选在步骤(iii)开始后3至7分钟,达到步骤(iv)中的所述时间“预定点”。
在本发明的实施方案中,一旦泡沫层的给定体积段达到50%至90%的固化度,优选地65%至85%的固化度,即达到步骤(iv)中的所述时间“预定点”。
本文使用的术语“固化度”是指通过傅里叶变换红外光谱(FTIR)测定的已反应的异氰酸酯基团的百分比,即100%的固化度表示基本上所有异氰酸酯(NCO)基团已发生反应,而0%的固化度表示基本上没有异氰酸酯(NCO)基团发生反应。
在生产复合材料的方法的不同阶段,NCO基团的量以及相应的固化度可以被原位监测(即沿着生产线,例如通过FTIR)。可以测量对应于0%固化度的NCO基团的数量,即可以在预聚物/前体组分混合之前,特别是与水混合之前,即在步骤(i)之前进行校准。
根据本发明使用的术语“完全固化”和“基本完全固化”是指90-100%的固化度。
在不希望受到理论约束的情况下,申请人认为,在实施加速固化步骤(iv)的整个固化工艺中,固化/交联反应已显著减弱,并且固化可通过均匀能量输入(即经由辐射,特别是经由IR辐射的能量输入)的方式有利地加速。通过选择由辐射输入产生的均匀加速,以及通过选择在其后大部分固化已经发生的时间点,在整个固化工艺的早期阶段可能发生的“失控”固化反应的风险被最小化或完全避免。
在本发明的实施方案中,步骤(iv)中沿着生产线的所述“预定位置”距离生产线中来自步骤(i)的混合物被施加到基底上的点(即“下游”)5m或更远,优选地10m或更远,进一步优选地20m或更远。
在本发明的实施方案中,在步骤(iv)中沿着生产线的所述“预定位置”在生产线的下游半部分[即,从生产线中来自步骤(i)的混合物施加到基底上的点进一步向下],优选在生产线的最后三分之一。
在本发明的实施方案中,通过步骤(iv)的加速固化在泡沫层表面达到的最高温度被控制在30℃至95℃的范围内,优选地45℃至90℃
在本发明的实施方案中,加速固化的区域,即步骤(iv)的区域在整个生产线的1m至10m范围内延伸,优选地在2m至6m范围内延伸。
在本发明的实施方案中,加速固化是通过提供沿生产线并朝向移动的泡沫层的至少2个IR灯来实现的,优选通过至少4个IR灯,进一步优选通过至少6个IR灯。
不希望被理论所束缚,申请人相信通过辐射加热,特别是UV加热(在100nm到350nm的波长范围内),IR加热(在700nm到1mm的波长范围内)或微波加热(在1mm到300mm的波长范围内)对于加速泡沫层的固化过程中的化学反应特别有利,因为这种辐射能够至少部分穿透泡沫层,然后被泡沫层内部吸收,从而通过不仅从外部提高温度,而且从内部提高温度来加速化学反应。
相比之下,通过对流或传导进行的常规加热,如通过常规加热方式实现的,例如在烘箱中,通过常规加热使泡沫层与热空气接触,这主要增加了来自外部的温度并导致温度梯度。在整个固化过程中固化已经减弱但没有停止或基本停止的阶段,引入这样的温度梯度可以导致沿着层的宽度和长度的固化梯度(外侧比内侧更多),这最终可以导致非均匀固化的泡沫层。此外,常规加热不仅加热泡沫,还加热周围区域,这需要热量控制。
因此,根据本发明,辐射加热允许加速整个固化过程,同时最小化沿泡沫层厚度或宽度的固化度的梯度。辐射加热还允许增加相对于对流加热/热空气加热/烘箱加热的响应时间。
辐射加速的这些优点尤其适用于聚氨酯基泡沫,因为它们的特点是导热性相对较差。
在本发明的优选实施方案中,步骤(iv)的加速固化通过用2个或更多个,优选4个或更多个IR灯进行红外加热来实现,进一步优选通过用4至10个IR灯进行红外加热来实现。在进一步的实施方案中,这些灯间隔开20cm至2m,优选40cm至100cm。发明人发现,通过将灯间隔得不太近,特别是通过将灯间隔在上述距离内,可以避免或最小化固化泡沫的过热。
(v)干燥步骤
在本发明的实施方案中,在步骤(iv)之后,该工艺包括另一个单独的干燥步骤(v)。
与步骤(iv)相反,所述干燥步骤的目的主要不是加速固化(“后固化”仍可能在所述干燥步骤期间发生),而是降低泡沫层中的含水量。
在本发明的实施方案中,在干燥步骤(v)之前,泡沫已经固化到至少90%,优选至少95%的程度。
在优选实施方案中,基本上固化的湿泡沫包含至少10%w/w的水、优选至少30%w/w的水、进一步优选至少50%w/w的水,并且干燥以达到等于或小于10%w/w、优选小于5%w/w、进一步优选小于2%w/w的预定含水量。
对于医疗应用中使用的泡沫,例如5%w/w的残余含水量通常被视为对泡沫性能有利。
在本发明的实施方案中,所述干燥步骤(v)中的温度(最高温度或平均温度,或两者)低于加速固化步骤(iv)中的温度。
在本发明的实施方案中,在步骤(v)中,通过对流和/或传导的常规加热被用作热能的主要来源,并且没有通过辐射提供额外的能量输入。
在本发明的实施方案中,在步骤(v)中通过干燥达到的最高温度在25℃至120℃的范围内,优选50℃至75℃。
根据本发明的第二方面,通过提供包含通过根据本发明的工艺获得或可获得的泡沫的伤口敷料来实现上述和其他目的。
在本发明的实施方案中,伤口敷料包括所述泡沫层,其中所述伤口敷料进一步包括至少一个另外的层,优选背衬层和/或粘合层或涂层,优选这些另外的层中的两个或更多个。
一般性定义
在权利要求中,术语“包含(comprising)”和“包含(comprise(s))”不排除其他元件或步骤,不定冠词“一(a)”或“一(an)”不排除多个元件或步骤。
在相互不同的从属权利要求中引用某些措施的事实并不表示这些措施的组合不能被有利地使用。
附图说明
现在将参照示出本发明示例性实施方案的附图,更详细地示出本发明的上述和其他方面,其中:
图1示出了整个生产线(1)的示意性和示例性草图,包括混合腔室(10),这里示例性地示出了三条进料线(11),用于施加泡沫层的装置,这里示例性地实现为喷嘴(12)基底(20),这里实现为移动输送带,泡沫层(21)从喷嘴分配到基底上,覆盖有可选的保护层(22),用于加速固化的区域(30),在此示例性地配备有三个IR灯(31),以及用于干燥泡沫的加热区域(40)。
图2示出了使用根据本发明的工艺制造的固化聚氨酯泡沫(21’)的示例性伤口敷料,所述伤口敷料包括背衬层(23)、所述固化泡沫层(21’)和伤口接触层(24)。在图2b中,所述伤口接触层显示为穿孔伤口接触层(24’)。
图3示出了沿着生产线的示例性温度分布的比较,示出了根据常规工艺(没有加速固化),以及根据本发明的示例性工艺使用六个IR灯的辐射加热,在基底(此处:纤维网)上的泡沫的温度分布(作为沿着图1所示生产线的位置的函数);温度的“峰值”很明显,但一旦IR加热被移除,温度基本上恢复到“正常”。
具体实施方式
在下面的进一步描述中,参考附图描述了本发明的详细实施方案,这些附图是本发明实施方案的示例性说明。
化学:
在本发明的实施方案中,预聚物是或包含异氰酸酯封端的多元醇或异氰酸酯封端的聚氨酯。
在本发明的实施方案中,预聚物来源于多元醇和二异氰酸酯化合物之间的反应,其中所述二异氰酸酯化合物选自六亚甲基二异氰酸酯(HDI)、甲苯二异氰酸酯(TDI)、亚甲基二苯基二异氰酸酯(MDI)或异佛尔酮二异氰酸酯(IPDI)或其任意混合物。
在本发明的实施方案中,预聚物来源于多元醇如聚乙二醇和六亚甲基二异氰酸酯(HDI)之间的反应。在本发明的实施方案中,预聚物是或包含六亚甲基异氰酸酯封端的多元醇,优选六亚甲基异氰酸酯封端聚乙二醇,或六亚甲基异氰酸酯封端聚氨酯。
在本发明的优选实施方案中,预聚物来源于多元醇和甲苯二异氰酸酯(TDI)之间的反应。在本发明的实施方案中,预聚物是或包含甲苯异氰酸酯封端多元醇,优选甲苯异氰酸酯封端聚乙二醇,或甲苯异氰酸酯封端聚氨酯。
在本发明的实施方案中,预聚物来源于多元醇和亚甲基二苯基二异氰酸酯(MDI)之间的反应。在本发明的实施方案中,预聚物是或包含亚甲基二苯基异氰酸酯封端多元醇,优选亚甲基二苯基异氰酸酯封端聚乙二醇,或亚甲基二苯基异氰酸酯封端聚氨酯。
在本发明的实施方案中,所述多元醇选自聚酯多元醇、聚丙烯酸酯多元醇、聚氨酯多元醇、聚碳酸酯多元醇、聚醚多元醇、聚酯聚丙烯酸酯多元醇、聚氨酯聚丙烯酸酯多元醇、聚氨酯聚酯多元醇、聚氨酯聚醚多元醇、聚氨酯聚碳酸酯多元醇和聚酯聚碳酸酯多元醇等,尤其是二元醇或任选的三元醇和四元醇以及二元羧酸或任选的三元羧酸和四元羧酸或羟基羧酸或内酯的缩聚物。
示例性合适的二醇是乙二醇、丁二醇、二甘醇、三甘醇、聚亚烷基二醇(比如聚乙二醇)以及1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇和异构体、新戊二醇或新戊二醇羟基新戊酸酯。此外,比如三羟甲基丙烷、甘油、赤藓糖醇、季戊四醇、三羟甲基苯或三羟乙基异氰脲酸酯等多元醇也在本发明的范围内。
在本发明的实施方案中,所述多元醇是聚乙二醇(聚环氧乙烷)。因此,在本发明的实施方案中,预聚物是或包含异氰酸酯封端聚乙二醇。
在本发明的实施方案中,二异氰酸酯化合物和多元醇的预聚物反应混合物中二异氰酸酯化合物的含量为至少15%(w/w)(相对于预聚物反应混合物中二异氰酸酯和多元醇的总重量)。在本发明的实施方案中,在二异氰酸酯化合物和多元醇的预聚物反应混合物中,二异氰酸酯化合物的含量为15-60%,优选20-50%(w/w)。
工艺条件
在本发明的实施方案中,整个工艺以这样的方式进行,使得泡沫层至少部分连续地被处理,特别是在步骤(ii)、(iii)和(iv)中或期间。
“至少部分连续”是指不包括任何仅分批或固定工艺。在上述工艺步骤中,至少在部分处理时间内,泡沫层沿着生产线连续输送。
在本发明的实施方案中,整个工艺是(仅)部分连续的,因为一个限定体积的起始材料将最终产生给定数量的泡沫卷,这些泡沫卷可以被储存并用于进一步的转化步骤(例如,涂覆硅酮和/或用作伤口衬垫中的层等)。
在本发明的实施方案中,本发明的工艺与沿着生产线的温度分布相关联,其中在加速步骤(iv)中实现最高总温度。
最终产品
在本发明的实施方案中,在步骤(iv)或步骤(v)之后得到的泡沫是开放孔泡沫,特别是具有至少50%的开孔,优选至少90%的开孔。如本文所用,术语“开放孔”指泡沫的孔结构,其中开放孔孔结构中的孔相互连接并形成互连网络。
在本发明的实施方案中,在步骤(iv)或步骤(v)之后产生的泡沫是开放孔泡沫,其具有平均尺寸在30μm到1000μm之间变化的孔。
根据本发明,“平均孔径”应理解为孔的(最大)横截面积,其中应用了孔的球形近似。通过泡沫材料的横截面的图像分析来测量孔径,其中图像分析方法基于ISO 13322-1:2014,并且相应地计算孔的横截面积。
在本发明的实施方案中,由步骤(iv)或步骤(v)产生的亲水性聚氨酯泡沫层是根据标准方法ISO 845:2006测量的密度为60至180kg/m3的开放孔多孔亲水性泡沫。
在本发明的实施方案中,泡沫层是一种开放孔多孔亲水性泡沫,其密度为60至180kg/m3,优选100至150kg/m3,根据标准方法ISO 845:2006进行测量。
在本发明的实施方案中,由步骤(iv)或步骤(v)产生的泡沫的厚度为500μm至20mm,优选为1mm至15mm。在本发明的实施方案中,泡沫层的厚度为1mm至12mm。在本发明的实施方案中,泡沫层的厚度为1mm至10mm。在本发明的实施方案中,泡沫层的厚度为1mm至8mm。在本发明的实施方案中,泡沫层的厚度为1mm至5mm。
在本发明的实施方案中,由步骤(iv)或步骤(v)得到的聚氨酯泡沫层是亲水性的。
根据本发明,术语“亲水性”应理解为在IUPAC中定义的:Compendium of ChemicalTerminology,第二版。(“Gold Book”),由A.D.McNaught和A.Wilkinson编纂。BlackwellScientific Publications,Oxford(1997),ISBN 0-9678550-9-8,一般指分子实体或取代基与极性溶剂,特别是水或其他极性基团相互作用的能力。
优选地,术语“亲水性”是指材料的透水性或分子的吸水性。对于具有孔的材料(这里是开放孔泡沫)或具有通孔的材料的情况下,如果该材料吸水,这种材料具有“亲水性”。
在本发明的实施方案中,泡沫材料的特征在于自由膨胀吸收能力,对应于EN13726-1:2002测量的最大吸收能力,为800至2500kg/m3。
在本发明的实施方案中,由步骤(iv)或步骤(v)产生的聚氨酯泡沫层具有至少5μl/sec、优选至少10μl/sec、更优选至少20μl/sec的吸收速度。
其他泡沫组分(抗菌)
在本发明的实施方案中,泡沫层包含抗菌剂。在本发明的实施方案中,抗菌剂包括银。在本发明的实施方案中,银是金属银。在本发明的实施方案中,银是银盐。在本发明的实施方案中,银盐是硫酸银、氯化银、硝酸银、磺胺嘧啶银、碳酸银、磷酸银、乳酸银、溴化银、乙酸银、柠檬酸银、CMC银、氧化银。在本发明的实施方案中,银盐是硫酸银。在本发明的实施方案中,抗菌剂包含单胍或双胍。在本发明的实施方案中,单胍或双胍是二葡萄糖酸氯己定、二醋酸氯己定、二盐酸氯己定、聚六亚甲基双胍(PHMB)或其盐,或聚六亚甲基单胍(PHMG)或其盐。在本发明的实施方案中,双胍是PHMB或其盐。在本发明的实施方案中,抗菌剂包括季铵化合物。在本发明的实施方案中,季铵化合物是西吡氯铵、苄索氯铵或聚-DADMAC。在本发明的实施方案中,抗菌剂包括三氯生、次氯酸钠、铜、过氧化氢、木糖醇或蜂蜜。本发明的优点已经在以下实施例中得到证明。
实施例
根据本发明实施方案的泡沫层是在标准实验室条件下制备的(除非另有说明,否则在室温下)。
通过以下步骤制备泡沫层:(1)将含有表面活性剂和可从Rynel Inc购得的预聚物的水相计量加入混合器中;(2)将水溶液和预聚物在针式混合器中混合,并分配在两个基底层之间;(3)然后将乳液混合物模压成一定的厚度和宽度;(4)泡沫在以固定线速度运行的移动输送机上自由固化;(5)大约四分钟后,用IR加热器(穿过基底层)加热反应泡沫乳液大约0.5分钟(24秒);(6)然后将纤维网(基底)移动到输送带的末端,在那里移除基底,将泡沫暴露于干燥步骤;在步骤(7)中,将成品泡沫收集到卷中并取样。
根据本发明示例性实施方案的这种方法能够比没有IR加热器的相同或类似工艺快大约25%的固化时间。在发现对泡沫性能影响极小甚至没有影响的同时,实现了工艺时间的优势。
Claims (15)
1.制造聚氨酯泡沫层的工艺,所述工艺至少包括以下步骤:
(i)至少一个混合步骤,其中一种或更多种聚氨酯预聚物或其前体在混合区域或接触区域中相互混合或接触,和/或与另一种组分混合或接触;
(ii)至少一个层形成步骤,其中来自步骤(i)的混合物被施加到移动的基底上以形成层并在基底上开始固化过程;
(iii)至少一个输送步骤,在该步骤中,来自步骤(ii)的基底上的泡沫层沿着生产线至少部分地移动,在该步骤中,泡沫层中的聚氨酯预聚物或其前体至少部分地固化,并且由于发泡,即由于在所述层中发生的至少一个化学反应,所述层的厚度增加;
(iv)至少一个加速固化的步骤,其在步骤(ii)结束后的时间预定点发生,并且相应地发生在沿着所述生产线的预定位置,其中通过使在基底上移动的泡沫经受辐射加热(优选红外辐射)来加速固化。
2.根据权利要求1所述的工艺,其中所述工艺包括至少进一步的步骤(v),其在步骤(iv)之后实施:
(v)与步骤(iv)分开并在其结束后:至少一个干燥步骤,在此期间,将来自步骤(iv)的基本固化的湿泡沫干燥以达到预定的较低含水量。
3.根据权利要求1或权利要求2所述的工艺,其中所述聚氨酯预聚物源自多元醇和二异氰酸酯化合物之间的反应,所述二异氰酸酯化合物选自六亚甲基二异氰酸酯(HDI)、甲苯二异氰酸酯(TDI)、亚甲基二苯基二异氰酸酯(MDI)或异佛尔酮二异氰酸酯(IPDI)或其任意混合物,优选甲苯二异氰酸酯(TDI)。
4.根据权利要求3所述的工艺,其中所述多元醇选自聚酯多元醇、聚丙烯酸酯多元醇、聚氨酯多元醇、聚碳酸酯多元醇、聚醚多元醇、聚酯聚丙烯酸酯多元醇、聚氨酯聚丙烯酸酯多元醇、聚氨酯聚酯多元醇、聚氨酯聚醚多元醇、聚氨酯聚碳酸酯多元醇和聚酯聚碳酸酯多元醇,尤其是二元醇或任选的三元醇和四元醇以及二元羧酸或任选的三元羧酸和四元羧酸或羟基羧酸或内酯的缩聚物。
5.根据前述权利要求中任一项所述的工艺,其中所述聚氨酯预聚物包含或为异氰酸酯封端多元醇或异氰酸酯封端聚氨酯。
6.根据前述权利要求中任一项所述的工艺,其中施加在基底上的泡沫层,即在在步骤(ii)开始时的泡沫层的初始厚度为100μm至8mm,优选250μm至2mm。
7.根据前述权利要求中任一项所述的工艺,其中(A)当泡沫的厚度相对于步骤(ii)中初始施加的层的厚度增加至少60%,优选至少80%时,或
(B)当达到泡沫固化的峰值温度时,优选当峰值温度已经过去时,或
(C)在步骤(iii)开始时温度在18℃至24℃、优选18℃至23℃的范围内之后,当泡沫层的温度在25℃至35℃、优选27℃至32℃的范围内时,
达到步骤(iv)中的所述时间“预定点”。
8.根据前述权利要求中任一项所述的工艺,其中步骤(iv)中的所述时间“预定点”在步骤(iii)开始后2至10分钟到达,优选在步骤(iii)开始后3至7分钟到达,或
其中一旦泡沫层的给定体积段达到50%至90%,优选65%至85%的固化度,就达到步骤(iv)中的所述时间“预定点”。
9.根据前述权利要求中任一项所述的工艺,其中步骤(iv)中沿生产线的所述“预定位置”距离所述生产线中将来自步骤(i)的混合物施加到基底上的点5m或更长,优选10m或更长,进一步优选20m或更长。
10.根据前述权利要求中任一项所述的工艺,其中通过步骤(iv)的加速固化达到的最高温度被控制在30℃到95℃的范围内,优选在45℃到90℃的范围内。
11.根据权利要求2至10中任一项所述的工艺,其中干燥步骤(v)中的最高温度或平均温度,优选两者,低于加速固化步骤(iv)中的温度。
12.根据前述权利要求中任一项所述的工艺,其中步骤(iv)或步骤(v)后产生的泡沫为开放孔泡沫,优选具有至少50%的开孔,优选至少90%的开孔。
13.根据前述权利要求中任一项所述的工艺,其中步骤(iv)的加速固化通过用2个或更多个,优选4个或更多个红外灯进行红外加热来实现,进一步优选其中所述灯间隔开20cm至2m,优选40cm至100cm。
14.一种医疗敷料,其包含根据权利要求1至13中任一项已获得或可获得的泡沫。
15.根据权利要求14所述的医疗敷料,其中所述医疗敷料进一步包括至少一个另外的层,优选背衬层和/或粘合层或涂层,优选这些另外的层中的两个或更多个。
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