CN113716934A - 一种柔韧性气凝胶复合绝热材料的制备工艺 - Google Patents
一种柔韧性气凝胶复合绝热材料的制备工艺 Download PDFInfo
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Abstract
本发明公开了一种柔韧性气凝胶复合绝热材料的制备工艺，包括以下步骤：（1）制备二氧化硅溶胶：将硅源、溶剂和水解催化剂混合水解；（2）复合：在二氧化硅溶胶中加入柔顺剂、凝胶催化剂，混合均匀，然后喷淋到基材中，使基材充满混合溶液；（3）成型：将复合完成后的材料输送到温度35‑45℃的条件下保持10‑30min，固定成型；（4）陈化：将成型的复合材料放入溶剂中浸泡；（5）疏水改性：将陈化后的复合材料放入改性液中浸泡；（6）干燥：采用超临界二氧化碳进行干燥。本发明制备出的柔韧性气凝胶复合绝热材料具有优良的保温、降噪、遮阳、防火性能，且施工方便；有效地缩短凝胶工艺时间、降低反应温度，简化工艺流程，生产可连续化，且生产成本低。
Description
技术领域
本发明属于化工材料技术领域，具体涉及一种柔韧性气凝胶复合绝热材料的制备工艺。
背景技术
目前的帐篷通常采用夹芯隔热材料通过降低热导率来达到保温的效果，包括纺织类隔热材料、建筑类隔热材料。因此，帐篷夹芯隔热材料及其技术的研究与开发是提高帐篷保温效果及实用性的重要途径。气凝胶是由胶体粒子或高聚物分子相互聚结构成纳米多孔网络结构，并在纳米孔隙中充满气态分散介质的一种高分散固态纳米材料，它具有低密度、高比表面积、低热导率、低声阻抗及低折射率、疏水且不然等特性。新型气凝胶隔热材料的热导率为0.014-0.022 W/m•K，低于纺织类隔热材料的热导率（0.035W/m•K），具有优异的保温隔热、隔音、轻质的特性。因此新型气凝胶隔热材料作为帐篷隔热夹芯材料具有巨大的优势和前景。以Aspen公司的SpaceloftR系列二氧化硅气凝胶复合材料产品为例，该产品的厚度为5～10 mm，密度为0.15 g/cm3，最高使用温度为200℃，同时具有疏水和阻燃的性能，常温热导率为0.014W/(m•K)，在隔热性能方面优于其他的隔热材料，其隔热性能优于其他一般隔热材料。但是目前的纤维增强氧化硅气凝胶隔热材料存在掉粉现象，难以承受反复弯折、折叠和重复使用。因此提高气凝胶复合材料的柔韧性、疏水性能，降低其制备成本具有十分重要的意义。
发明内容
为解决上述问题，本发明的目的是提供一种柔韧性气凝胶复合绝热材料的制备工艺。
一种柔韧性气凝胶复合绝热材料的制备工艺，包括以下步骤：
（1）制备二氧化硅溶胶：将硅源、溶剂和水解催化剂按照1：（1-9）：（0.001-0.005）的体积比例混合，温度为20-60℃，搅拌时间为2-6h，水解得到二氧化硅溶胶；所述硅源包括正硅酸甲酯、正硅酸乙酯、聚多硅氧烷中一种或两种以上混合物：所述溶剂包括甲醇、丙醇、乙醇、丙酮中的一种或两种以上的组合；所述水解催化剂包括纯水、盐酸、硫酸、硝酸、草酸中一种或两种以上的组合；
（2）复合：将二氧化硅溶液输送到缓冲罐中加热至30-60℃，然后再与柔顺剂、凝胶催化剂在管道内混合，然后喷淋到基材中，使基材充满混合溶液；所述二氧化硅溶胶、柔顺剂、凝胶催化剂的体积比例为1：（0.025-0.2）：（0.05-0.2），所述柔顺剂为乙烯基三甲氧基硅烷、甲基三甲氧基硅烷、乙烯基三乙氧基硅烷、甲基三乙氧基硅烷、乙烯基聚二基甲硅氧烷中一种或两种以上的组合，所述凝胶催化剂为氨水、氟化铵、碳酸铵、乙二胺、碳酸氢铵、氢氧化钠中的一种或两种以上的组合，所述基材为碳纤维、聚酯纤维、超细纤维、芳纶纤维中的一种；
（3）成型：将复合完成后的材料输送到温度35- 45℃的条件下保持10-30min，使凝胶与基材溶为一体，固定成型；
（4）陈化：将成型的复合材料放入浸泡液中，于20-60℃浸泡5-48h；
（5）疏水改性：将陈化后的复合材料放入改性液中浸泡5-48h，改性液是将表面改性剂和溶剂按照体积比1:（50-150）的体积比例混合而成，改性温度为20-60℃，所述表面改性剂包括六甲基二硅氮烷、六甲基二硅氧烷、三甲基氯硅烷中一种或两种以上的组合；
（6）干燥：采用超临界二氧化碳进行干燥，温度为45-55℃，压力为10-16MPa，二氧化碳的流量为1800-3000kg/h，干燥时间为6-12h。
本发明柔韧性气凝胶复合绝热材料的制备工艺，与现有技术相比，其有益效果在于：1.本发明制备出的柔韧性气凝胶复合绝热材料具有优良的保温性能、降噪性能、遮阳性能、防火性能，且施工方便；2. 本发明有效地缩短凝胶工艺时间、降低反应温度，简化工艺流程，操作简易，生产可连续化，且生产成本低。
附图说明
下面结合附图对本发明做进一步详细说明。
图1为本发明制备出的柔韧性气凝胶复合绝热材料；
图2为本发明制备出的柔韧性气凝胶复合绝热材料对折时的示意图；
图3为本发明制备出的柔韧性气凝胶复合绝热材料卷曲时的示意图；
图4为本发明制备出的柔韧性气凝胶复合绝热材料对折后卷曲的示意图；
图5为本发明制备出的柔韧性气凝胶复合绝热材料的导热系数测试曲线。
具体实施方式
以下由特定的具体实施例说明本发明的实施方式，熟悉此技术的人士可由本说明书所揭露的内容轻易地了解本发明的其他优点及功效。
实施例1
一种柔韧性气凝胶复合绝热材料的制备工艺，包括以下步骤：
（1）制备二氧化硅溶胶：将正硅酸乙酯、甲醇、乙醇、水和盐酸按照1：5.5:1.5:0.147:0.004的体积比例混合，具体的甲醇为工业甲醇，乙醇为无水乙醇，在45℃温度条件下搅拌为3h，水解得到二氧化硅溶胶；
（2）复合：将二氧化硅溶液输送到缓冲罐中加热至30℃，然后按照二氧化硅溶胶：乙烯基三乙氧基硅烷：氨水溶液=1： 0.025： 0.05的体积比例，在管道内混合，然后喷淋到芳纶纤维中，使芳纶纤维充满混合溶液；
（3）成型：将复合完成后的材料输送到温度35℃的条件下保持15min，使凝胶与基材溶为一体，固定成型；
（4）陈化：将成型的复合材料放入甲醇中，于60℃浸泡24h；
（5）疏水改性：将陈化后的复合材料放入改性液中浸泡10h，改性液是将六甲基二硅氮烷和甲醇按照体积比1: 100的体积比例混合而成，改性温度为60℃；
（6）干燥：采用超临界二氧化碳进行干燥，温度为45℃，压力为16MPa，二氧化碳的流量为1800kg/h，干燥时间为8h，干燥釜下方的排液口无溶液排出，停机取出二氧化硅气凝胶复合材料。
随机选取测量密度为221.6kg/m3，常温导热系数0.017W/m• K，燃烧等级为A级不燃。
实施例2
一种柔韧性气凝胶复合绝热材料的制备工艺，包括以下步骤：
（1）制备二氧化硅溶胶：将正硅酸乙酯、甲醇、乙醇、水和盐酸按照1：5.5:1.5:0.147:0.004的体积比例混合，具体的甲醇为工业甲醇，乙醇为无水乙醇，盐酸为浓盐酸，在50℃温度条件下搅拌为3h，水解得到二氧化硅溶胶；
（2）复合：将二氧化硅溶液输送到缓冲罐中加热至40℃，然后按照二氧化硅溶胶：乙烯基三乙氧基硅烷：氨水溶液=1：0.05：0.06的体积比，在管道内混合，然后喷淋到芳纶纤维中，使芳纶纤维充满混合溶液；
（3）成型：将复合完成后的材料输送到温度40℃的条件下保持10min，使凝胶与基材溶为一体，固定成型；
（4）陈化：将成型的复合材料放入甲醇中，于55℃浸泡24h；
（5）疏水改性：将陈化后的复合材料放入改性液中浸泡10h，改性液是将六甲基二硅氮烷和甲醇按照体积比1:150的体积比例混合而成，改性温度为55℃；
（6）干燥：采用超临界二氧化碳进行干燥，温度为50℃，压力为14MPa，二氧化碳的流量为2000kg/h，干燥时间为7h，干燥釜下方的排液口无溶液排出，停机取出二氧化硅气凝胶复合材料。
随机选取测量密度为208.8kg/ m3，常温导热系数0.0165W/m• K，燃烧等级为A级不燃。
本发明制备出的气凝胶复合绝热材料的照片参见图1；本发明制备出的柔韧性气凝胶复合绝热材料对折时的照片参见图2；本发明制备出的柔韧性气凝胶复合绝热材料卷曲时的照片参见图3；本发明制备出的柔韧性气凝胶复合绝热材料对折后卷曲的照片参见图4；本发明制备出的柔韧性气凝胶复合绝热材料的导热系数测试曲线参见图5，其中横坐标为记录次数，纵坐标为导热系数。
本发明的保护范围不限于具体实施方式所公开的技术方案，凡是依据本发明的技术实质对以上实施例所作的任何修改、等同替换、改进等，均落入本发明的保护范围。
Claims (7)
1.一种柔韧性气凝胶复合绝热材料的制备工艺，其特征在于: 包括以下步骤：
（1）制备二氧化硅溶胶：将硅源、溶剂和水解催化剂按照1：（1-9）：（0.001-0.005）的体积比例混合，搅拌水解得到二氧化硅溶胶；
（2）复合：在二氧化硅溶胶中加入柔顺剂、凝胶催化剂，混合均匀，然后喷淋到基材中，使基材充满混合溶液；
（3）成型：将复合完成后的材料输送到温度35- 45℃的条件下保持10-30min，使凝胶与基材溶为一体，固定成型；
（4）陈化：将成型的复合材料放入溶剂中浸泡；
（5）疏水改性：将陈化后的复合材料放入改性液中浸泡；
（6）干燥：采用超临界二氧化碳进行干燥。
2.如权利要求1所述的柔韧性气凝胶复合绝热材料的制备工艺，其特征在于:所述步骤（1）中制备二氧化硅溶胶时的温度为20-60℃，搅拌时间为2-6h。
3. 如权利要求1或2所述的柔韧性气凝胶复合绝热材料的制备工艺，其特征在于: 所述硅源包括正硅酸甲酯、正硅酸乙酯、聚多硅氧烷中一种或两种以上混合物：所述溶剂包括甲醇、丙醇、乙醇、丙酮中的一种或两种以上的组合；所述水解催化剂包括纯水、盐酸、硫酸、硝酸、草酸中一种或两种以上的组合。
4.如权利要求3所述的柔韧性气凝胶复合绝热材料的制备工艺，其特征在于:所述复合是将二氧化硅溶液输送到缓冲罐中加热至30-60℃，然后再与柔顺剂、凝胶催化剂在管道内混合，所述二氧化硅溶胶、柔顺剂、凝胶催化剂的体积比例为1：（0.025-0.2）：（0.05-0.2），所述柔顺剂为乙烯基三甲氧基硅烷、甲基三甲氧基硅烷、乙烯基三乙氧基硅烷、甲基三乙氧基硅烷、乙烯基聚二基甲硅氧烷中一种或两种以上的组合，所述凝胶催化剂为氨水、氟化铵、碳酸铵、乙二胺、碳酸氢铵、氢氧化钠中的一种或两种以上的组合，所述基材为碳纤维、聚酯纤维、超细纤维、芳纶纤维中的一种。
5. 如权利要求4所述的柔韧性气凝胶复合绝热材料的制备工艺，其特征在于: 所述陈化是将成型的复合材料放入溶剂中，于20-60℃浸泡5-48h。
6.如权利要求5所述的柔韧性气凝胶复合绝热材料的制备工艺，其特征在于:所述改性液是将表面改性剂和溶剂按照体积比1:（50-150）的体积比例混合而成，改性时温度为20-60℃，改性时浸泡时间为5-48h，所述表面改性剂包括六甲基二硅氮烷、六甲基二硅氧烷、三甲基氯硅烷中一种或两种以上的组合。
7.如权利要求6所述的柔韧性气凝胶复合绝热材料的制备工艺，其特征在于:所述干燥时，温度为45-55℃，压力为10-16MPa，二氧化碳的流量为1800-3000kg/h，干燥时间为6-12h。
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