CN114889252B - 一种气凝胶-双组分针刺纤维毡的复合材料及其制备方法和应用 - Google Patents

一种气凝胶-双组分针刺纤维毡的复合材料及其制备方法和应用 Download PDF

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CN114889252B
CN114889252B CN202210468041.8A CN202210468041A CN114889252B CN 114889252 B CN114889252 B CN 114889252B CN 202210468041 A CN202210468041 A CN 202210468041A CN 114889252 B CN114889252 B CN 114889252B
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张秋华
卫荣辉
陈翔
陈文军
赵真真
饶良波
刘平
江小华
谭堂航
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Guangdong Ellison Technology Co ltd
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Abstract

本发明属于隔热材料技术领域，公开了一种气凝胶‑双组分针刺毡的复合材料及其制备方法和应用。所述复合材料依次包括保冷层、粘结层和防水层，所述的保冷层为气凝胶包覆双组分针刺纤维毡的隔热材料，所述粘结层为热熔胶膜，所述防水层为铝箔复合膜。该复合材料中气凝胶均匀的分布在双组分针刺纤维毡里外周围，一体成型结构的隔热性能稳定均匀，生成的隔热材料质量稳定和可控，且不会受外界振动或运输运行等影响隔热材料的品质，可广泛应用在保冷领域中。

Description

一种气凝胶-双组分针刺纤维毡的复合材料及其制备方法和应用
技术领域
本发明属于隔热材料技术领域，更具体地，涉及一种气凝胶-双组分针刺纤维毡的复合材料及其制备方法和应用。
背景技术
气凝胶是一种很好的隔热材料，用于保温和保冷均具有高效的绝热效果，最常用的使用方式是用气凝胶与增强纤维制成复合材料，能更好的满足应用部位的使用要求。在用于保冷领域时，因气凝胶多孔特性，在冷环境下可能会因冷凝液吸入容易冻结，需要对保冷下的防水进行强化处理，一是自身具备憎水功能；二是要对多孔的特点进行强化防护。同时，在天然气及液氮等冷环境的应用场景下，还需考虑一些安全保障因素，如防火预防，兼顾二氧化硅气凝胶自身的优势特性。因此，应注重各层结构材料的特性来发挥强化的保冷用气凝胶-双组分针刺毡复合材料的综合特性。在气凝胶制品隔热材料中，很多是通过成品简单的材料1+1+1等的模式形成结构组合材料，这样让隔热材料的保冷性能会出现明显差异。因此，需考虑气凝胶制品材料中通过在气凝胶制备生成过程中加入需复合的制品材料，让两者形成完整的均匀混合体对发挥气凝胶材料高效隔热性能具有显著优势。现有技术中生成气凝胶颗粒填充或粘结在纤维层上，这样形成的质量随时可能会受到多因素影响品质。比如，在保冷使用过程中，若是振动厉害，溶液导致填充或粘结的气凝胶颗粒和纤维层分离。
发明内容
为了解决上述现有技术的不足，本发明首要目的在于提供了一种气凝胶-双组分针刺毡的复合材料。该复合材料中气凝胶均匀的分布在双组分针刺纤维毡里外周围，一体成型结构的隔热性能稳定均匀，生成的隔热材料质量稳定和可控，且不会受外界振动或运输运行等影响隔热材料的品质。
本发明的另一目的在于提供上述气凝胶-双组分针刺毡的复合材料的制备方法。
本发明的再一目的在于提供上述气凝胶-双组分针刺毡的复合材料的应用。
本发明的目的通过下述技术方案来实现：
一种气凝胶-双组分针刺纤维毡复合材料，所述复合材料依次包括保冷层、粘结层和防水层，所述的保冷层为气凝胶包覆双组分针刺纤维毡的隔热材料，所述粘结层为热熔胶膜，所述防水层为铝箔复合膜。
优选地，所述保冷层、粘结层和防水层的厚度分别为1～12mm，0.01～0.25mm和0.01～1mm。
优选地，所述隔热材料包括20～80wt％的气凝胶和20～80wt％的双组分针刺纤维毡；所述双组分针刺毡是由无机纤维和阻燃合成纤维组成。
更为优选地，所述无机纤维为玻璃纤维或/和岩棉；所述阻燃合成纤维为聚酯纤维、聚酰胺纤维、聚丙烯腈纤维、聚氨酯弹性纤维中的一种以上。
优选地，所述热熔胶膜为EVA胶膜、PA胶膜、PES胶膜、PO胶膜、TPU胶膜中的一种以上。
所述的气凝胶-双组分针刺纤维毡复合材料的制备方法，包括如下具体步骤：
S1.将含硅化合物、溶剂、水和助剂形成均匀混合液，加入酸催化剂和碱催化剂，制得硅溶胶液；
S2.将硅溶胶液加入铺展双组分针刺纤维毡的浸胶槽中，保持硅溶胶液没过双组分针刺纤维毡表层，使硅溶胶液均匀的浸润双组分针刺纤维毡，形成复合体；
S3.将复合体置于密闭空间内在10～50℃进行凝胶化，形成凝胶化复合体，静置老化4～96h后，采用超临界CO2流体干燥，然后置于有机硅烷蒸汽中修饰改性，得到气凝胶包覆双组分针刺纤维毡的隔热材料；
S4.将气凝胶包覆双组分针刺纤维毡的隔热材料置于热压设备平台上，将热熔胶膜覆盖在隔热材料的表面，再将铝箔复合膜覆盖在热熔胶膜的表面，将上述整体在100～220℃经热轧辊热压后，除去毛刺和表面除尘冷却后，制得气凝胶-双组分针刺纤维毡复合材料。
优选地，步骤S1中所述含硅化合物为正硅酸乙酯或/和正硅酸甲酯；所述的溶剂为乙醇或/和甲醇；所述助剂为硅烷偶联剂、钛酸丁酯、含钛白或炭黑的醇溶液；所述含硅化合物、溶剂、水和助剂的摩尔比为1:(3～25):(1～5):(0.005～0.6)。
优选地，步骤S1中所述酸催化剂为醋酸、柠檬酸、氢氟酸、草酸、硝酸或盐酸中的一种以上；所述碱催化剂为氨水或/和氟化铵，所述酸催化剂、碱催化剂和含硅化合物的摩尔比为(0.001～0.02):(0.001～0.02):1；所述含钛白或炭黑的醇溶液中醇为乙醇或甲醇；所述钛白为醇的5～20wt％，炭黑为醇的5～10wt％。
优选地，步骤S3中所述有机硅烷蒸汽为三甲基乙氧基硅烷、六甲基二硅氮烷、二甲基硅油、辛基硅烷、三甲基二乙氧基硅烷中的一种以上。
所述的气凝胶-双组分针刺毡复合材料在保冷领域中的应用。
本发明的防水层可改变气凝胶多孔透气易吸潮的不足，防水层选材上兼顾考虑其需具备一定阻燃防火作用，并采用合适的胶膜能够通过遇热熔融下将防水层与气凝胶制品隔热材料很好的粘结形成完整的复合体材料。考虑到在冷环境下，增强纤维既要兼顾冷环境下的良好优势，比如采用合成纤维，但单纯的合成纤维，通常是高分子化合物组成的，其自身的阻燃防火性没有无机材料好，其复合气凝胶量会收到一定限制。因此，考虑采用无机纤维混合合成纤维的组分即保持了冷环境下的优势又能提高阻燃防火性，同时由于双组分纤维的差别液能提高复合气凝胶后的结构力。
与现有的技术对比，本发明有以下的有益效果：
1.本发明采用原位复合法先将气凝胶在生成之前即溶胶阶段原位复合双组分纤维针刺毡，再生成气凝胶-双组分针刺纤维毡的隔热材料，气凝胶均匀的分布在双组分针刺纤维毡里外周围，一体成型结构的隔热性能稳定均匀，生成的隔热材料的质量稳定和可控，且不会受外界振动或运输运行等影响隔热材料的品质。制得的隔热材料振动质量损失率小于1％，在气凝胶复合绝热制品的振动质量损失范围内，不会影响产品质量。参照国家标准GB/T 34336《纳米孔气凝胶复合绝热制品》振动质量损失率应不大于1％。同时，气凝胶原位复合在纤维上，不会因为单层的材料缺陷而导致隔热层失效。
2.本发明采用双组分针刺纤维毡，充分利用了双组分纤维的优势特点，比如玻璃纤维等无机纤维具有很好的防火性，密度通常高于合成纤维，没有合成纤维那么柔韧，耐高温，用来提高保冷层的阻燃性和结构力；合成纤维具有一定的阻燃性，密度比较轻，比较轻柔，但在低温下的保冷性能比较好，所以合成纤维与无机纤维结合成双组分，使得气凝胶复合双组分针刺纤维毡形成的隔热材料很好的发挥保冷层的保冷作用。
3.本发明在保冷层自身具备憎水防水性能下，为了避免气凝胶多孔特性在保冷长期湿环境下的长期寿命即避免一切可能的冻结因素，通过增加一层防水层材料来预防气凝胶多孔特性的冻结的潜在失效风险，相当于保冷层外增加了一层”保护外衣“来保护发挥主体保冷隔热功能的隔热层，让保冷层的保冷隔热功能发挥长期高效作用。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.取4mm厚的玻璃纤维-聚丙烯腈纤维双组分针刺纤维毡整齐铺展在浸胶槽；
2.将正硅酸乙酯、乙醇、水和含5wt％的炭黑乙醇溶液按摩尔比1：13：4：0.007充分搅拌形成混合液，再依次加入草酸和氨水(草酸：氨水：正硅酸乙酯的摩尔比为0.01：0.01：1)的进一步搅拌均匀，搅拌均匀后形成硅溶胶液；
3.将硅溶胶液均匀的浸渗在步骤1中玻璃纤维-聚丙烯腈纤维双组分针刺纤维毡上，待硅溶胶液液面没过针刺纤维毡表层后停止浸渗，浸渗均匀后形成了复合体，将其转移至轨道箱内密闭在25℃下进行凝胶化，约30min后形成凝胶化复合体。
4.待凝胶化复合体老化48h后，在90℃、15MPa条件下进行超临界CO2流体干燥5h，干燥后置于充满六甲基二硅氮烷蒸汽的改性修饰2h，得到气凝胶包覆双组分针刺纤维毡的隔热材料。
5.将气凝胶包覆双组分针刺纤维毡的隔热材料铺展在热压设备传送平台上，将0.1mm的PES胶膜下表面覆盖在气凝胶包覆双组分针刺纤维毡的隔热材料表层上，将0.25mm厚的铝箔布覆盖在PES胶膜表面上，合并后置于130℃加热箱，用热轧辊热压后输出，再经过切割机去除复合材料边沿外的毛刺和多余的铝箔布等；将边沿修饰后的材料进入表面吸尘设备内进行表面除尘和吹风冷却后，制得气凝胶-双组分针刺纤维毡的复合材料。
本实施例所得的气凝胶包覆双组分针刺纤维毡的隔热材料经测试在25℃下导热系数为0.0178，0℃下导热系数为0.0172，憎水率为99.5％；所得气凝胶-双组分针刺毡的复合材料，水蒸气吸收率小于5％，振动质量损失率小于1％，燃烧性能测试为不燃。
实施例2
1.取6mm厚的玻璃纤维-聚酯纤维双组分针刺纤维毡整齐铺展在浸胶槽；
2.将正硅酸乙酯、乙醇、水和KH550硅烷偶联剂按摩尔比1：15：3：0.01充分搅拌形成混合液，再依次加入盐酸和氨水(盐酸：氨水：正硅酸乙酯的摩尔比为0.005：0.01：1)的进一步搅拌均匀，搅拌均匀后形成硅溶胶液；
3.将硅溶胶液均匀的浸渗在步骤1中玻璃纤维-聚酯纤维双组分针刺纤维毡上，待硅溶胶液液面没过玻璃纤维-聚酯纤维双组分针刺纤维毡表层后停止浸渗，浸渗均匀后形成了复合体，将转移至轨道箱内密闭在20℃下进行凝胶化，约50min后形成凝胶化复合体。
4.待凝胶化复合体老化36h后，在90℃、15MPa条件下进行超临界CO2流体干燥5h，干燥后置于充满三甲基乙氧基硅烷蒸汽中修饰2h，得到气凝胶包覆双组分针刺纤维毡的隔热材料。
5.将气凝胶包覆双组分针刺纤维毡的隔热材料铺展在热压设备传送平台上，将0.15mmTPU胶膜覆盖在气凝胶包覆双组分针刺纤维毡的隔热材料表层上，将0.25mm厚的铝箔布覆盖在TPU胶膜表面上，合并后置于100℃加热箱，用热轧辊热压后输出，再经过切割机去除复合材料边沿外的毛刺和多余的铝箔布等；将边沿修饰后的材料进入表面吸尘设备内进行表面除尘和吹风冷却后，制得气凝胶-双组分针刺纤维毡的复合材料。
本实施例所得的气凝胶包覆双组分针刺纤维毡的隔热材料经测试在25℃下导热系数为0.0168，0℃下导热系数为0.0165，憎水率为99.7％；所得气凝胶-双组分针刺毡的复合材料，水蒸气吸收率小于5％，振动质量损失率小于1％，燃烧性能测试为不燃。
实施例3
1.取12mm厚的岩棉-聚酯纤维双组分针刺纤维毡整齐铺展在浸胶槽；
2.将正硅酸乙酯、乙醇、水与含10wt％钛白的甲醇溶液按摩尔比1：7：5：0.5充分搅拌形成混合液，再依次加入硝酸和氨水(硝酸：氨水：正硅酸乙酯的摩尔比为0.005：0.008：1)的进一步搅拌均匀，搅拌均匀后形成硅溶胶液；
3.将硅溶胶液均匀的浸渗在步骤1中岩棉-聚酯纤维双组分针刺纤维毡上，待硅溶胶液液面没过针刺纤维毡表层后停止浸渗，浸渗均匀后形成了复合体，将转移至轨道箱内密闭在30℃下进行凝胶化，约45min后形成凝胶化复合体。
4.待凝胶化复合体老化96h后，在90℃、15MPa条件下进行超临界CO2流体干燥5h，干燥后置于充满三甲基二乙氧基硅烷蒸汽中修饰2h，得到气凝胶包覆双组分针刺纤维毡的隔热材料。
5.将气凝胶包覆双组分针刺纤维毡的隔热材料铺展在热压设备传送平台上，将0.2mmEVA胶膜覆盖在气凝胶包覆双组分针刺纤维毡的隔热材料的表层上，将0.5mm厚的铝箔布覆盖在EVA胶膜表面上，合并后置于100℃加热箱，用热轧辊热压后输出，再经过切割机去除复合材料边沿外的毛刺和多余的铝箔布等；将边沿修饰后的材料进入表面吸尘设备内进行表面除尘和吹风冷却后，制得气凝胶-双组分针刺纤维毡的复合材料。
本实施例所得的气凝胶包覆双组分针刺纤维毡的隔热材料经测试在25℃下导热系数为0.0170，0℃下导热系数为0.0166，憎水率为99.8％；所得气凝胶-双组分针刺毡的复合材料，水蒸气吸收率小于5％，振动质量损失率小于1％，燃烧性能测试为不燃。
本发明实施例所得的气凝胶包覆双组分针刺纤维毡的隔热材料经测试在25℃下导热系数为0.0168～0.0170，0℃下导热系数为0.0165～0.0166，憎水率为99％以上；所得气凝胶-双组分针刺毡的复合材料，水蒸气吸收率小于5％，振动质量损失率小于1％，燃烧性能测试为不燃。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (8)

1.一种气凝胶-双组分针刺纤维毡复合材料，其特征在于，所述复合材料依次包括保冷层、粘结层和防水层，所述的保冷层为气凝胶包覆双组分针刺纤维毡的隔热材料，所述粘结层为热熔胶膜，所述防水层为铝箔复合膜；所述隔热材料包括20~80wt%的气凝胶和20~80wt%的双组分针刺纤维毡；所述双组分针刺纤维毡是由无机纤维和阻燃合成纤维组成；所述无机纤维为玻璃纤维或/和岩棉；所述阻燃合成纤维为聚酯纤维、聚酰胺纤维、聚丙烯腈纤维、聚氨酯弹性纤维中的一种以上；
其中，所述的气凝胶-双组分针刺纤维毡复合材料的制备方法，包括如下具体步骤：
S1. 将含硅化合物、溶剂、水和助剂形成均匀混合液，加入酸催化剂和碱催化剂，制得硅溶胶液；所述含硅化合物为正硅酸乙酯或/和正硅酸甲酯；所述的溶剂为乙醇或/和甲醇；所述助剂为硅烷偶联剂、钛酸丁酯、含钛白或炭黑的醇溶液；所述含硅化合物、溶剂、水和助剂的摩尔比为1:（3~25）:（1~5）:（0.005~0.6）；
S2. 将硅溶胶液加入铺展双组分针刺纤维毡的浸胶槽中，保持硅溶胶液没过双组分针刺纤维毡表层，使硅溶胶液均匀的浸润双组分针刺纤维毡，形成复合体；
S3. 将复合体置于密闭空间内在10~50℃进行凝胶化，形成凝胶化复合体，静置老化4~96h后，采用超临界CO2流体干燥，然后置于有机硅烷蒸汽中修饰改性，得到气凝胶包覆双组分针刺纤维毡的隔热材料；
S4. 将气凝胶包覆双组分针刺纤维毡的隔热材料置于热压设备平台上，将热熔胶膜覆盖在隔热材料的表面，再将铝箔复合膜覆盖在热熔胶膜的表面，将上述整体在100~220℃经热轧辊热压后，除去毛刺和表面除尘冷却后，制得气凝胶-双组分针刺纤维毡复合材料。
2.根据权利要求1所述的气凝胶-双组分针刺纤维毡复合材料，其特征在于，所述保冷层、粘结层和防水层的厚度分别为1~12mm，0.01~0.25mm和0.01~1mm。
3.根据权利要求1所述的气凝胶-双组分针刺纤维毡的复合材料，其特征在于，所述热熔胶膜为EVA胶膜、PA胶膜、PES胶膜、PO胶膜、TPU胶膜中的一种以上。
4.根据权利要求1-3任一项所述的气凝胶-双组分针刺纤维毡复合材料的制备方法，其特征在于，包括如下具体步骤：
S1. 将含硅化合物、溶剂、水和助剂形成均匀混合液，加入酸催化剂和碱催化剂，制得硅溶胶液；
S2. 将硅溶胶液加入铺展双组分针刺纤维毡的浸胶槽中，保持硅溶胶液没过双组分针刺纤维毡表层，使硅溶胶液均匀的浸润双组分针刺纤维毡，形成复合体；
S3. 将复合体置于密闭空间内在10~50℃进行凝胶化，形成凝胶化复合体，静置老化4~96h后，采用超临界CO2流体干燥，然后置于有机硅烷蒸汽中修饰改性，得到气凝胶包覆双组分针刺纤维毡的隔热材料；
S4. 将气凝胶包覆双组分针刺纤维毡的隔热材料置于热压设备平台上，将热熔胶膜覆盖在隔热材料的表面，再将铝箔复合膜覆盖在热熔胶膜的表面，将上述整体在100~220℃经热轧辊热压后，除去毛刺和表面除尘冷却后，制得气凝胶-双组分针刺纤维毡复合材料。
5.根据权利要求4所述的气凝胶-双组分针刺纤维毡复合材料的制备方法，其特征在于，步骤S1中所述含硅化合物为正硅酸乙酯或/和正硅酸甲酯；所述的溶剂为乙醇或/和甲醇；所述助剂为硅烷偶联剂、钛酸丁酯、含钛白或炭黑的醇溶液；所述含硅化合物、溶剂、水和助剂的摩尔比为1:（3~25）:（1~5）:（0.005~0.6）。
6.根据权利要求4所述的气凝胶-双组分针刺纤维毡复合材料的制备方法，其特征在于，步骤S1中所述酸催化剂为醋酸、柠檬酸、氢氟酸、草酸、硝酸或盐酸中的一种以上；所述碱催化剂为氨水或/和氟化铵，所述酸催化剂、碱催化剂和含硅化合物的摩尔比为（0.001~0.02）:（0.001~0.02）:1；所述含钛白或炭黑的醇溶液中醇为乙醇或甲醇；所述钛白为醇的5~20wt%，炭黑为醇的5~10wt%。
7.根据权利要求4所述的气凝胶-双组分针刺纤维毡复合材料的制备方法，其特征在于，步骤S3中所述有机硅烷蒸汽为三甲基乙氧基硅烷、六甲基二硅氮烷、二甲基硅油、辛基硅烷中的一种以上。
8.权利要求1-3任一项所述的气凝胶-双组分针刺毡复合材料在保冷领域中的应用。
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