CN101115817B - 用于热量管理的相变材料（pcm）组合物 - Google Patents

用于热量管理的相变材料（pcm）组合物 Download PDF

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CN101115817B
CN101115817B CN2005800479903A CN200580047990A CN101115817B CN 101115817 B CN101115817 B CN 101115817B CN 2005800479903 A CN2005800479903 A CN 2005800479903A CN 200580047990 A CN200580047990 A CN 200580047990A CN 101115817 B CN101115817 B CN 101115817B
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composition
pcm
weight
phase change
deck
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CN101115817A (zh
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L·P·罗兰
R·J·C·赖斯多夫
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EIDP Inc
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EI Du Pont de Nemours and Co
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Abstract

本发明涉及相变材料(PCM)组合物，所述组合物包含a)20-80％重量PCM；和b)20-80％重量一种或多种选自如下的聚合物：b1)按照ASTM 792测定的密度等于或低于0.910g/cm3的极低密度聚乙烯(VLDPE)；b2)按照ASTM 792测定的密度等于或低于0.900g/cm3的乙丙橡胶(EPR)；b3)苯乙烯-乙烯-丁二烯-苯乙烯(SEBS)共聚物；和b4)苯乙烯-丁二烯-苯乙烯(SBS)共聚物。本发明PCM组合物可用于需要热量管理的应用，例如建筑、汽车、包装、服装和鞋类。

Description

用于热量管理的相变材料(PCM)组合物
发明领域
本发明涉及用于建筑、汽车、包装、服装和鞋类等不同领域进行热量管理的相变材料(PCM)组合物。本发明还涉及包含上述PCM组合物的片材和模制品。
发明背景
所有技术领域中存在一个普遍需要：能量有效。例如建筑业中，永远需要降低与加热和冷却室内空间有关的能量成本。这对纺织业同样如此，如生物和个人防护服，其中必须将穿着者产生过剩热从其身体移走、管理，以提高总体穿着舒适性。
PCM材料为高产储热介质，它能分别吸收和释放熔融和结晶过程大量的潜热。这种相变过程中，PCM材料的温度基本保持不变且PCM周围空间的温度也是如此，流经PCM的热量被“束缚”在PCM本身内。已知石蜡作为PCM特别有效。
图1显示了典型夏天(纬度：45°；经度：180°；空气Tmin：15℃；空气Tmax：35℃)中三种建筑墙结构(木材结构)内表面温度分布模拟。这三种墙结构包括外层(木披迭板，厚度：20mm)，紧挨着该外层的岩棉层(厚度：250mm)和内灰泥板(厚度：10mm)。第一种墙结构(W1)不包含PCM，而第二种和第三种墙结构(W2；W3)还包含位于岩棉层和灰泥板层之间的PCM组合物层，所述PCM组合物层分别由7.15％重量PCM与92.85％重量假想聚合物和45％重量PCM与55％重量假想聚合物组成。该模拟考虑的PCM产自Rubitherm，商品名为Rubitherm
Figure G05847990320070813D000011
RT20(熔点：22℃)。
图1表明：白天内墙温度变量随着墙结构中PCM量增加而减小，或换句话说，墙结构的热量管理性能随着其中包含的PCM量增加而提高。
WO 2004/044345公开了包含结晶烷基烃等相变材料作为储热设施的外墙组合体。该组合体包括：1)被乙烯基涂层覆盖的织物或纸覆盖层；2)由丙烯酸类涂层化合物组成的中间层(包含磨碎的PCM)和由液态陶瓷化合物组成、使用过程朝着墙的后层。然而由于丙烯酸类材料本身的极性和较高结晶度，丙烯酸类涂层结合PCM的能力是有限的，从而整个组合体的储热能力只能达到一受限程度。
US 5,053,446公开了用于热能储存的复合材料，所述复合材料为其中结合有PCM(例如结晶烷基烃)的聚烯烃基体。所述聚烯烃基体是结晶的且在高达150-180℃必须是形态热稳定的。这是由于基体的PCM吸收(imbibition)必须在高达上述值的温度下进行，以使得PCM材料本身渗透到结晶基体的狭窄空间。通常通过在吸收之前使得聚烯烃形成网络来实现热稳定。这对于制备复合材料而言是附加的步骤，该附加步骤使得整个生产过程更复杂和昂贵。此外，由于基体本身内空间有限，正确保留PCM(特别是在低于PCM熔点的温度下)是非常困难的，这导致整个复合材料的热量管理性能大大下降。
因此本发明根本问题是提供在建筑、汽车、服装和鞋类等不同应用中进行热量管理的PCM组合物，所述PCM组合物可克服上述问题。
发明概述
目前惊人地发现：通过PCM组合物可克服上述问题，所述PCM组合物包含：
a)20-80％重量PCM；和
b)20-80％重量一种或多种选自如下的聚合物：
b1)按照ASTM 792测定的密度等于或低于0.910g/cm3的极低密度聚乙烯(VLDPE)；
b2)按照ASTM 792测定的密度等于或低于0.900g/cm3的乙丙橡胶(EPR)；
b3)苯乙烯-乙烯-丁二烯-苯乙烯(SEBS)共聚物；和
b4)苯乙烯-丁二烯-苯乙烯(SBS)共聚物；
所述百分重量以组合物总重计。
本发明另一方面提供采用上述PCM组合物制备的片材及包括所述片材的多层结构。
本发明还一方面提供由上述PCM组合物制备的模制品。
附图简述
图1为典型夏天中三种建筑墙结构(木材结构)内表面温度分布模拟(纬度：45°；经度：180°；空气Tmin：15℃；空气Tmax：35℃)。
发明详述
本发明中所用的聚合物具有低极性和结晶度。聚合物的低极性对于使得聚合物本身和非极性PCM之间相容非常重要。此外，由于其无定形，用于本发明的聚合物基体具有足够吸收能力以结合和保留大量PCM，即使在高于或低于PCM本身的熔点的温度下也是如此。上述聚合物有效地将PCM保留在其基体内的能力赋予本发明组合物长期优异热量管理性能。
聚合物密度与结晶百分比按照以下等式(D.Campbell和J.R.White，Polymer Characterization，Chapman and Hall，1989，第328页)直接相关：
                ％结晶度＝ρs-ρa/ρc-ρa
其中ρs是给定聚合物的密度，ρa是具有无定形结构的同一聚合物的密度而ρc是具有100％结晶结构的相同聚合物的密度。
就本发明而言，所述一种或多种聚合物可选自所有类型的SEBS和SBS共聚物，众所周知所述共聚物是无定形的且通常密度为0.900-1.1g/cm3。也可能采用密度等于或低于0.900g/cm3的EPR和密度等于或低于0.910g/cm3，优选0.800-0.910g/cm3的VLDPE，所有密度按照ASTM 792测定。
本发明优选实施方案中，PCM组合物包含EPR，所述EPR选自乙烯-丙烯-二烯-亚甲基(EPDM)、乙烯-丙烯-亚甲基(EPM)及其混合物。或者用于本发明PCM组合物的唯一聚合物为密度等于或低于0.910g/cm3的VLDPE。
有利地是，本发明的PCM组合物包含30-50％重量且更优选约40％总量的一种或多种聚合物，所述重量百分比以PCM组合物总重计。
本发明优选实施方案中，PCM选自一种或多种烷基烃(石蜡)。石蜡是饱和烃混合物且通常由化学式为CH3-(CH2)n-CH3的基本直链n-烷烃的混合物组成。-(CH2)n-链的结晶释放大量潜热。熔点和熔化热随着链长增加而提高。因此，可能按照一定方式选择石蜡(其为石油精炼产物)使得相变温度范围符合采用PCM的操作系统的温度。
将三种不同石蜡的热性能列于表1中。
                     表1
  烷烃  C数   熔点℃   熔化热KJ/kg  比热CpKJ/kg℃   RT状态
  十四烷  14   5.8   227  2.18   液态
  十五烷  15   9.9   206   液态
  十六烷  16   18.1   236  2.22   固态
优选本发明PCM组合物包含50-70％重量PCM，优选60％重量，重量百分比以PCM组合物总重计。
另一实施方案中，本发明PCM组合物还包含约10-40％重量惰性粉末，所述惰性粉末的吸收容量为至少50％重量且优选至少120％重量，所述重量百分比以惰性粉末本身的干重计。使用惰性粉末还提高了PCM在聚合物基体中的保留量。有利地是用于本发明PCM组合物的惰性粉末为硅酸盐、一种或多种阻燃填充剂及其混合物。所述一种或多种阻燃填充剂有利地选自氢氧化铝、氢氧化镁、蜜胺焦磷酸盐、蜜胺氰尿酸盐、一种或多种溴化填充剂及其混合物。
本发明另一方面，PCM组合物的一种或多种聚合物接枝有0.2-3％重量的羧酸或羧酸酐官能团，所述重量百分比以所述一种或多种聚合物总重计。尽管这样少量羧酸或羧酸酐不影响聚合物基体的总极性，如果PCM组合物与例如铝箔组合使用，则希望这种官能团以上述量存在，这是由于羧酸或羧酸酐官能度大大改善PCM组合物对金属表面的粘附力。
可通过本领域中已知的任何常规方法(例如采用硅烷和/或过氧化物基交联剂)使本发明PCM组合物的聚合物基体在将PCM结合到其中后交联。在此过程中，重要的是避免PCM发生交联。可例如通过在结合PCM之前将硅烷基接枝到聚合物分子上得以实现。这种接枝可通过常规技术进行，例如通过在加入0.2-2％重量乙烯基-三甲氧基硅烷或乙烯基-三乙氧基硅烷与0.05-0.5％重量过氧化物后将聚合物在超过150℃下挤出。然后可将PCM结合到硅烷接枝聚合物，所得混合物可在水或湿气存在下通过采用月桂酸二丁基锡等催化剂交联。当用于下列不同应用中时聚合物基体的这种交联能提高组合物本身的力学和热性能。
本发明PCM组合物可还包含抗氧剂和UV过滤剂等常规添加剂。组合物中这些添加剂的量和状态在本领域中是总所周知的。
本发明PCM组合物可通过在稍微高于PCM熔点但低于所述一种或多种聚合物熔点的温度下将不同组分一起浸渍来制备。浸渍是熔融PCM被聚合物基体自然吸收。通常在桶混机中将各组分混合一段时间，所述时间可随着桶混机本身的旋转速度变化。通常时间为约8小时。
得到本发明PCM组合物的另一种可能是通过熔融混合物挤出，其中各组分在高于所述一种或多种聚合物和PCM熔点的温度下混合，由此所得的混合物随后被挤出成粒或直接成为片材或任何合适形式。
采用上述PCM组合物制备的片材也是本发明的目标。优选这种片材的厚度为0.5-10mm且通过如上所述的熔融混合物挤出来直接制备，或通过制备PCM组合物，随后通过例如挤出、压延和热层合等任何常规技术对所述组合物进行加工来制备。
本发明另一目标是多层结构，所述多层结构包含上述PCM组合物的至少一片材(A)，所述片材与至少一层(B)相邻。优选这种片材(A)位于两层(B1，B2)之间。所述至少一层(B)或优选两层(B1，B2)的一个作用是帮助将片材(A)的PCM材料包含在聚合物基体内，从而能较长时间保持片材(A)的PCM的热量管理性能处于较高水平。此外这样避免了与PCM组合物相邻的表面上的不需要润滑油污。
本发明一个实施方案中，多层结构包含以如下顺序的各构成：
a)至少一片材(A)；
b)与所述至少一片材(A)相邻的至少一层(B)；
c)与所述至少一层(B)相邻的一层或多层附加层(C)。
本发明另一实施方案中，多层结构还包含与层(B1，B2)的一层或多层相邻并在其外面的一层或多层附加层(C)。
所述至少一层(B)和所述一层或多层附加层(C)也可具有赋予整个多层结构改进的阻燃性和导热性的作用，从而容易将热通过这种至少一层传递到PCM组合物且反之亦然。
所述至少一层(B)和所述一层或多层附加层(C)可由铝组成。也可使用在一面采用铝真空涂布的聚酯，所述铝化面面对PCM片材(A)以实现最佳粘合。使用铝化聚酯还赋予整个PCM多层结构优异的力学强度及优异的弹性。
根据具体用途和应用，所述至少一层(B)和所述一层或多层附加层(C)可由其它材料而不是上述铝和/或聚酯真空涂布材料组成或由其它材料与上述铝和/或聚酯真空涂布材料一起组成。这种材料可独立选自一种或多种阻燃聚合物组合物(用氢氧化铝、氢氧化镁、碳酸钙等阻燃无机填充剂、溴化填充剂和蜜胺焦磷酸盐填充的聚合物)、石膏(石膏板)、岩棉绝缘材料、玻璃棉绝缘材料、泡沫聚苯乙烯和通常用于建筑业的其它材料。
根据所用材料，所述至少一层(B)和所述一层或多层附加层(C)厚度可为5μm-20cm。例如铝层厚度一般为5-500μm，优选20-80μm且更优选约50μm。
可采用常规方法制备本发明多层结构。这包括将PCM材料挤出涂布到所述至少一层(B)，将PCM材料挤出层合到两层(B1，B2)之间和将PCM材料和所述至少一层(B)共挤出(如果这种至少一层(B)的材料可进行这样的操作(例如如果所述至少一层由阻燃组合物组成))。
本发明另一方面涉及由上述PCM组合物组成的模制品。这种模制品可通过适合使得热塑性材料变形的任何方法(包括注塑法、吹塑法、热成型和滚塑法)制备。
本发明PCM组合物可用于需要热量管理的多种应用。尽管建筑物内的温度管理是一种最相关的应用，本发明PCM组合物也可用于汽车应用(例如车辆车顶、车座和轮胎)、空气管道中的空气过滤器、运输应用、食品包装(保持食品冷却或温热)、药物包装、服装和运动服用机织和无纺织布、鞋类、树包裹物、手柄(工具、运动产品和车辆中的)、垫褥、毛毯、木质复合材料、电缆和热介质(包括水)用热塑料管。
将在以下实施例中对本发明进一步描述。
实施例
实施例1
将55g产自Rubitherm、商品名为RubithermRT20的石蜡(PCM，熔点为22℃)和45g产自E.I.du Pont de Nemours and Company、商品名为Fusabond
Figure G05847990320070813D000072
493D的与0.5％重量马来酸酐接枝的VLDPE粒子(密度为0.863g/cm3)同时引入1升桶混机。在25℃下混合8小时以有足够时间来将液态石蜡最大量结合到聚合物基体中(浸渍)。将用石蜡浸渍的粒子从混合器中取出并过滤以从其外表面除去剩余的液态石蜡。测量浸润之前或之后粒子重量的差异，从而可计算被聚合物基体吸收的石蜡重量百分比。
将以上得到的PCM组合物压模来制备板材。将粒子放在2块钢板之间的框(厚度为2mm)中且随后在夹片温度为100℃和压力为1bar下将整个系统挤压1分钟并在随后的2分钟内在80bar下挤压。然后在4分钟内将夹片冷却到25℃，保持压力为80bar。最终释放压力并将得到的聚合物板从框中移出。
对模制板的柔韧性进行测试。还按照方法DIN 53504S2在从两块这种板切出的哑铃状条样品上对拉伸强度和断裂伸长进行测试。
将结果显示于表2中。
实施例2(对比)
采用产自E.I.du Pont de Nemours and Company、商品名为Elvaloy
Figure G05847990320070813D000081
AC 1125的乙烯-丙烯酸甲酯粒子(包含25％重量丙烯酸甲酯)重复实施例1。实施例2中没有采用得到的PCM组合物制备板。
将结果显示于表2中。
实施例3
采用产自Dow Chemicals、商品名为Engage
Figure G05847990320070813D000082
8180的VLDPE粒子(密度为0.863g/cm3)重复实施例1。实施例3中没有采用得到的PCM组合物制备板。
将结果显示于表2中。
实施例4(对比)
采用产自E.I.du Pont de Nemours and Company、商品名为DuPontTM6611的HDPE粒子(密度为0.965g/cm3)重复实施例1。实施例4中没有采用得到的PCM组合物制备板。
将结果显示于表2中。
实施例5(对比)
采用产自E.I.du Pont de Nemours and Company、商品名为DuPontTM6611的HDPE粒子(密度为0.965g/cm3)重复实施例1。在180℃混合8小时。
将结果显示于表2中。
表2
 实施例1  实施例2  实施例3  实施例4  实施例5
 浸渍温度(℃)  25  25  25  25  180
 重量％1  100  23  100  13  100
 模制板的柔韧性  非常柔韧  非常柔韧  非常脆
 拉伸强度(MPa)  ＞4.62  2.1
 断裂伸长(％)  ＞22932  5.9
1 8小时浸润后被聚合物基体吸收的石蜡的重量百分比，100％表示全部吸收，即55g石蜡被吸收到45g聚合物中。
2 2293％(4.6Mpa)是采用测试设备可测量的最大值。
表2表明在25℃下本发明聚合物基体(实施例1和3)可吸收全部量(每45g聚合物55g PCM)，而具有高极性(实施例2)或高结晶度(实施例4)的聚合物仅能有限量地吸收PCM。为了采用高结晶度HDPE基体实现PCM的完全吸收，需要将浸润温度提高到180℃(实施例5)。将本发明PCM组合物模塑得到的板非常柔韧且显示出优异力学性能。另一方面，实施例5表明采用基于结晶聚合物(HDPE)的PCM组合物制备的板非常脆。因此，从力学方面考虑，这种组合物即使其PCM含量非常高，也不适用于热量管理应用。
实施例6
在220℃下，将44.6g产自Dow Chemical、商品名为Engage
Figure G05847990320070813D000101
8180的VLDPE粒子(密度为0.863g/cm3)和0.4g乙烯基三甲氧基硅烷和过氧化物催化剂的混合物(XL-Pearl
Figure G05847990320070813D000102
23，产自General Electric，OsiSpecialities)挤出得到混合物。将55g产自Rubitherm、商品名为RubithermRT20的55g石蜡(PCM)(熔点为22℃)、0.03g月桂酸二丁基锡和45g以上得到的VLDPE基混合物同时引入1升桶混机。在25℃下混合8小时以有足够时间来将液态石蜡和月桂酸二丁基锡最大量结合到聚合物基体中(浸渍)。将用石蜡和月桂酸二丁基锡浸渍的粒子从混合器中取出。
将本实施例6及实施例3中得到PCM组合物压模来制备板材。将粒子放在2块钢板之间的框(厚度为2mm)中且随后在夹片温度为100℃下和压力为1bar下将整个系统挤压第1分钟并在随后的2分钟内在80bar下挤压。然后在4分钟内将夹片冷却到25℃，保持压力为80bar。最终释放压力并将得到的聚合物板从框中移出。然后将所得板材浸入水中4小时并按照方法DIN 53504S2从这些板材切出哑铃状条样品。
将52g砝码悬挂到固定在烘箱内的各哑铃状条上。在不同温度下测试15分钟。记录各样品断裂的温度。将结果显示于表3中。
表3
 实施例3  实施例6
  样品断裂温度(℃)  40  80
表3表明：与相同未交联组合物(实施例3)相比，实施例6中得到的交联组合物具有明显改进的耐热变形性能。

Claims (11)

1.一种相变材料组合物，所述组合物包含：
a)50-70%重量的一种或多种石蜡；和
b)30-50%重量的一种或多种选自如下的聚合物：
按照ASTM 792测定的密度等于或低于0.910g/cm3的极低密度聚乙烯，其任选接枝0.2至3%重量的羧酸或羧酸酐官能团，所述重量百分数基于所述一种或多种聚合物的总重量计算；
所述百分重量以组合物总重计，
其中所述相变材料组合物还包含10-40%重量的惰性粉末，所述惰性粉末的吸收容量为至少50%重量，所述重量百分比以惰性粉末的干重计，其中所述惰性粉末为硅酸盐、一种或多种阻燃填充剂及其混合物。
2.权利要求1的相变材料组合物，其中所述惰性粉末的吸收容量为至少120%重量，所述重量百分比以惰性粉末的干重计。
3.权利要求1的相变材料组合物，其中所述一种或多种阻燃填充剂选自氢氧化铝、氢氧化镁、蜜胺焦磷酸盐、蜜胺氰尿酸盐、一种或多种溴化填充剂及其混合物。
4.权利要求1的相变材料组合物，所述组合物还包含抗氧剂和UV过滤剂。
5.权利要求1的相变材料组合物，其中所述一种或多种聚合物是交联的聚合物。
6.一种采用权利要求1的相变材料组合物制备的柔韧性片材。
7.一种多层结构，所述多层结构包含至少一层权利要求6的柔韧性片材A，所述柔韧性片材A与至少一层B相邻，所述至少一层B由选自以下的材料制备：铝、用铝真空涂布的聚酯、一种或多种阻燃聚合物组合物、石膏、岩棉绝缘材料、玻璃棉绝缘材料和泡沫聚苯乙烯。
8.权利要求7的多层结构，其中所述至少一柔韧性片材A位于所述至少一层B的两层B1、B2之间，所述两层独立由选自以下的材料制备：铝、用铝真空涂布的聚酯、一种或多种阻燃聚合物组合物、石膏、岩棉绝缘材料、玻璃棉绝缘材料和泡沫聚苯乙烯。
9.权利要求8的多层结构，所述多层结构包含如下顺序的各构件：
a)至少一柔韧性片材A；
b)与所述至少一柔韧性片材A相邻的至少一层B；
c)与所述至少一层B相邻的一层或多层附加层C，所述一层或多层附加层C独立由选自以下的材料制备：铝、用铝真空涂布的聚酯、一种或多种阻燃聚合物组合物、石膏、岩棉绝缘材料、玻璃棉绝缘材料和泡沫聚苯乙烯。
10.权利要求9的多层结构，所述多层结构还包含与所述至少一层B的两层B1、B2的一层或多层相邻并在其外面的一层或多层附加层C，所述一层或多层附加层C独立由选自以下的材料制备：铝、用铝真空涂布的聚酯、一种或多种阻燃聚合物组合物、石膏、岩棉绝缘材料、玻璃棉绝缘材料和泡沫聚苯乙烯。
11.一种由权利要求1的相变材料组合物制成的模塑部件。
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