CN111335024B - 一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法 - Google Patents
一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法 Download PDFInfo
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Abstract
本发明公开了一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法，包括如下步骤，S1)将非金属晶体矿物熔融提纯，添加稀有金属化合物，制成耐高温纤维；S2)开松将耐高温纤维梳理成厚度均匀的薄棉网；S3)在薄棉网上施加耐溶剂胶水原液烘干脱水制成耐溶剂耐高温孔棉，经连续化生产制成耐高温纤维无纺布卷材；S4)将绝热粉末均匀分散在100%醇类溶剂里，形成混合溶液，在抽真空混合釜内将耐高温纤维无纺布卷材浸泡在混合溶液中，进行还原逆反应；S5)采用低温真空离心法回收反应残留的醇类溶剂，制得成品无纺布，本发明所制备无纺布超薄、超轻，耐高温1000℃，绝热，耐受浓度100%醇类溶剂，具有出色的干态湿态强度，保持结构完整，可电气绝缘，可防爆。
Description
技术领域
本发明涉及功能性无纺布技术领域，尤其涉及一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法。
背景技术
绝热材料是指能阻滞热流传递的材料，又称热绝缘材料。传统绝热材料，如玻璃纤维、聚氨酯泡棉、岩棉、硅酸盐等；新型绝热材料，如气凝胶毡、真空板等，它们是用于建筑围护或者热工设备、阻抗热流传递的材料或者材料复合体，既包括保温材料，也包括保冷材料。绝热材料一方面满足了建筑空间或热工设备的储热环境，另一方面在新能源交通工具的热管理和安全防护领域也起到关键作用。因此，有些国家将绝热材料看作是继风能、太阳能、核能、生物质能之后的“第五大清洁能源”。
绝热材料，如无碱玻璃纤维制品等，软化点在600℃，无法在高温1000℃长期使用；碳纤维制品，耐温可达1000℃，但无法在存在电源放电的环境使用；芳纶制品，对位芳纶1414的耐温500℃，无法在高温1000℃长期使用，而且价格又相对昂贵；岩棉制品，室温下导热系数大概0.03W/(m·k)，绝热性不错，但绝热防护时太厚太占用空间，无法使用在小型移动设备领域，且耐侯性不佳，在日常环境中使用两年就需要局部更换。
绝热功能也可以通过绝热涂料涂层来实现，最好的绝热涂料可以耐高温1000℃，但一旦绝热涂料涂层被烧穿，底层的支撑体就会被快速烧毁，使用时只能喷涂在支撑体上，经过6到8小时的自然固化后涂层才能和支撑体牢固地结合，工艺时间太长而无法连续化生产。
发明内容
本发明的目的在于提供一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法，以解决上述背景技术中所提出的问题。
为达到上述目的，本发明采用的技术方案是：一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法，包括如下步骤，
S1)将非金属晶体矿物经高温1500℃熔融提纯，添加稀有金属化合物，经离心甩丝法制成耐高温纤维；
S2)通过物理开松将耐高温纤维梳理成厚度均匀的薄棉网；
S3)在薄棉网上施加耐溶剂胶水原液，根据不同的施胶工艺，施胶量为4％-12％，胶水原液经过高温反应聚合成可以耐受高浓度醇类溶剂的分子量2万到20万之间的大分子基团，二者经温度160℃-190℃烘干脱水制成耐溶剂耐高温孔棉，在高温脱除水分的过程中，薄棉网与胶水原液由交联化学反应被粘结成型，且胶水原液聚合成大分子基团，经连续化生产制成耐高温纤维无纺布卷材；
S4)将绝热粉末均匀分散在100％醇类溶剂里，形成混合溶液，在抽真空混合釜内将耐高温纤维无纺布卷材浸泡在混合溶液中，经还原逆反应，使绝热粉末渗透共混填充满耐高温纤维无纺布的网络空隙间；
S5)采用低温真空离心法回收反应残留的醇类溶剂，制得成品无纺布。
作为进一步的优化，所述稀有金属化合物为含钛、锂、钨、钼、锆、钒元素化合物中的一种或者几种，添加稀有金属化合物可进一步活化熔融体所制晶体纤维的长期耐高温性能。
作为进一步的优化，所述耐高温纤维为石英纤维、S级玻璃纤维、高硅氧纤维、二氧化硅纤维、硅酸铝纤维、陶瓷纤维、氧化铝纤维、氧化锆纤维、岩棉、玄武岩纤维、云母纤维中的一种或者几种。
作为进一步的优化，所述耐高温纤维的直径不小于4μm，其长度不小于1mm。
作为进一步的优化，所述耐溶剂胶水原液由水性改性树脂与软水复配制成，其含固量为25％-60％，所述水性改性树脂为环氧改性聚氨酯树脂、环氧改性聚丙烯酸酯树脂、环氧改性乙烯基树脂、环氧树脂、丁苯橡胶、丁腈橡胶、顺丁橡胶、异戊橡胶、硅橡胶、氟橡胶中的一种或者几种。
作为进一步的优化，所述耐溶剂耐高温孔棉的网隙率大于60％。
作为进一步的优化，S3)中施胶工艺为浸渍法、喷淋法、真空抽吸法、平板式浸轧法、凹版转移涂胶法、圆网转移涂胶法的一种。
作为进一步的优化，所述绝热粉末为氧化铝、氧化硅、二氧化硅、二氧化钼、氧化铁、氧化锆、碳化硅、硅酸铝、氧化钛、氧化钼气凝胶粉中的一种或者几种。
作为进一步的优化，所述醇类溶剂为甲醇、乙醇、乙二醇、丙醇、正丁醇、异丁醇、正戊醇、异戊醇、正己醇、异己醇中的一种或几种。
与现有技术相比，本发明的有益效果是：
1.本发明将刚性的耐高温纤维加工成型成可弯曲、可对折、不折断的柔性无纺布卷材；
2.本发明无纺布在浓度100％醇类小分子量溶剂内浸泡3小时后，横向/纵向湿强度不低于干强度的90％；在浓度100％醇类小分子量溶剂内浸泡24小时后，横向/纵向湿强度不低于干强度的75％，尺寸型变量小于等于10％；
3.无纺布厚度小于等于5mm，0.5mm-2mm无纺布的厚度公差小于等于10％，2mm-5mm无纺布的厚度公差小于等于5％；
4.可连续化生产，无纺布每卷长度大于等于100米；
5.无纺布耐高温1000℃长期使用，且无纺布经受高温1000℃/冲击压强0.5兆帕的火焰持续喷燃5min后没有烧穿或形变；
6.无纺布导热系数小于等于0.02W/(m·k)；
7.无纺布使用过程中没有胶粒或粉末析出；
8.无纺布使用年限不低于10年；
9.可连续化生产，依托节能、环保、绿色的无纺布生产工艺，生产效率高，能耗低，产量高(单线产能可达1.8万延米/天)，交付快。
附图说明
图1为本发明的扫描电镜图(放大倍数500倍)。
图2为本发明的截面图。
图3为本发明的成品状态示意图。
具体实施方式
以下是本发明的具体实施例，对本发明的技术方案作进一步的描述，但本发明并不限于这些实施例。
实施例1
一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法，包括如下步骤，
S1)将非金属晶体矿物经高温1500℃熔融提纯，添加稀有金属锆化合物(质量浓度1.0％)和金属锂化合物(质量浓度0.3％)，经离心甩丝法制成直径为7μm、长度4mm的S级玻璃纤维，可成型为耐高温纤维；
S2)通过物理开松将耐高温纤维梳理成2mm厚度均匀的薄棉网；
S3)在薄棉网上采用凹版转移涂胶法施加耐溶剂胶水原液，耐溶剂胶水原液由水性环氧改性聚氨酯树脂与软水复配制成，二者质量溶度分别为50％和50％，施胶量为6％，胶水原液经过高温反应聚合成可以耐受高浓度醇类溶剂的分子量2万到20万之间的大分子基团，二者经温度160℃烘干脱水制成耐溶剂耐高温孔棉，在高温脱除水分的过程中，薄棉网与胶水原液由交联化学反应被粘结成型，且胶水原液聚合成大分子基团，耐溶剂耐高温孔棉孔隙率为60％，经连续化生产制成耐高温纤维无纺布卷材；
S4)将氧化锆气凝胶绝热粉末均匀分散在100％异戊醇溶剂里，形成混合溶液，在抽真空混合釜内将耐高温纤维无纺布卷材浸泡在混合溶液中，进行还原逆反应，使绝热粉末渗透共混填充满耐高温纤维无纺布的网络空隙间；
S5)采用低温真空离心法回收反应残留的醇类溶剂，制得成品无纺布。
实施例2
一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法，包括如下步骤，
S1)将非金属晶体矿物经高温1500℃熔融提纯，添加稀有金属钛化合物(质量浓度0.5％)和金属钼化合物(质量浓度0.3％)，经离心甩丝法制成纤维直径为11μm、长度6mm的玄武岩纤维，可成型为耐高温纤维；
S2)通过物理开松将耐高温纤维梳理成5mm厚度均匀的薄棉网；
S3)在薄棉网上采用平板式浸轧法施加耐溶剂胶水原液，耐溶剂胶水原液由水性顺丁橡胶、水性硅橡胶与软水复配制成，三者质量溶度分别为10％、25％和65％，施胶量为10％，胶水原液经过高温反应聚合成可以耐受高浓度醇类溶剂的分子量2万到20万之间的大分子基团，二者经温度190℃烘干脱水制成耐溶剂耐高温孔棉，在高温脱除水分的过程中，薄棉网与胶水原液由交联化学反应被粘结成型，且胶水原液聚合成大分子基团，耐溶剂耐高温孔棉的网隙率为70％，经连续化生产制成耐高温纤维无纺布卷材；
S4)将氧化铝气凝胶绝热粉末均匀分散在100％正丁醇溶剂里，形成混合溶液，在抽真空混合釜内将耐高温纤维无纺布卷材浸泡在混合溶液中，进行还原逆反应，使绝热粉末渗透共混填充满耐高温纤维无纺布的网络空隙间；
S5)采用低温真空离心法回收反应残留的醇类溶剂，制得成品无纺布。
实施例3
一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法，包括如下步骤，
S1)将非金属晶体矿物经高温1500℃熔融提纯，添加稀有金属锆化合物(质量浓度1.0％)和金属锂化合物(质量浓度0.3％)，经离心甩丝法制成直径7μm、长度4mm的S级玻璃纤维，与直径9μm和长度6mm的二氧化硅纤维，二者按照纤维重量比50％和50％混合成耐高温纤维组合料；
S2)通过物理开松将耐高温纤维组合料梳理成3mm厚度均匀的薄棉网；
S3)在薄棉网上采用真空吸胶法施加耐溶剂胶水原液，耐溶剂胶水原液由水性丁苯橡胶、水性环氧改性乙烯基树脂与软水复配制成(复配质量溶度比例为30％、15％和55％)，施胶量为6％，胶水原液经过高温反应聚合成可以耐受高浓度醇类溶剂的分子量2万到20万之间的大分子基团，二者经温度180℃烘干脱水制成耐溶剂耐高温孔棉，在高温脱除水分的过程中，薄棉网与胶水原液由交联化学反应被粘结成型，且胶水原液聚合成大分子基团，耐溶剂耐高温孔棉的网隙率为65％，经连续化生产制成耐高温纤维无纺布卷材；
S4)将二氧化钼气凝胶绝热粉末均匀分散在100％丙醇溶剂里，形成混合溶液，在抽真空混合釜内将耐高温纤维无纺布卷材浸泡在混合溶液中，进行还原逆反应，使绝热粉末渗透共混填充满耐高温纤维无纺布的网络空隙间；
S5)采用低温真空离心法回收反应残留的醇类溶剂，制得成品无纺布。
应用实施例：
对本发明无纺布的各指标进行测试，并与常规绝热材料进行对比，其结果如下表所示，
通过实验数据可知，本发明无纺布具有如下优点：
1.超薄，厚度5mm无纺布的绝热性能优于厚度20mm岩棉保温毡；2.超轻，厚度3mm无纺布的容重为200kg/m3，比铝合金轻1/12，比碳钢轻1/28；3.耐高温1000℃，耐温比铝合金高70％，比聚酰亚胺(PI)、聚醚醚酮(PEEK)、聚苯硫醚(PPS)等特种工程塑料高60％，比无碱玻璃纤维还高40％；4.绝热，室温下绝热性能等同于空气的导热系数0.02W/(m·k)；5.耐溶剂，耐受溶度100％醇类溶剂浸泡，出色的干湿态强度，保持结构完整；6.电气绝缘，非金属耐高温棉、有机耐溶剂胶、无机绝热粉末的电阻率都超过1x1012欧姆·厘米；7.连续化生产，依托节能、环保、绿色的无纺布生产工艺，生产效率高，能耗低，产量高(单线产能可达1.8万延米/天)，交付快；8.防爆，承受0.5Mpa的冲击压强持续5分钟，没有结构破坏。
本文中所描述的具体实施例仅仅是对本发明作举例说明。本发明所属技术领域的技术人员可以对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，但并不会偏离本发明的精神或者超越所附权利要求书所定义的范围。
Claims (7)
1.一种超薄耐1000℃绝热绝缘柔性无纺布的制备方法，其特征在于，包括如下步骤，
S1)将非金属晶体矿物经熔融提纯，添加稀有金属化合物，经离心甩丝法制成耐高温纤维；
S2)通过物理开松将耐高温纤维梳理成厚度均匀的薄棉网；
S3)在薄棉网上施加耐溶剂胶水原液，经烘干脱水制成耐溶剂耐高温孔棉，连续生产制成耐高温纤维无纺布卷材，施胶量为4%-12%，烘干温度为160℃-190℃，其中，所述耐溶剂胶水原液的含固量为25%-60%，其由水性改性树脂与软水复配制成，所述水性改性树脂为环氧改性聚氨酯树脂、环氧改性聚丙烯酸酯树脂、环氧改性乙烯基树脂、环氧树脂、丁苯橡胶、丁腈橡胶、顺丁橡胶、异戊橡胶、硅橡胶、氟橡胶中的一种或者几种，所述耐溶剂耐高温孔棉的网隙率大于60%；
S4)将绝热粉末均匀分散在浓度100%醇类溶剂里，形成混合溶液，在抽真空混合釜内将耐高温纤维无纺布卷材浸泡在混合溶液中，进行还原逆反应；
S5)采用低温真空离心法回收反应残留的醇类溶剂，制得成品无纺布。
2.根据权利要求1所述的超薄耐1000℃绝热绝缘柔性无纺布的制备方法，其特征在于，所述稀有金属化合物为含钛、锂、钨、钼、锆、钒元素化合物中的一种或者几种。
3.根据权利要求1所述的超薄耐1000℃绝热绝缘柔性无纺布的制备方法，其特征在于，所述耐高温纤维为石英纤维、S级玻璃纤维、高硅氧纤维、二氧化硅纤维、硅酸铝纤维、氧化铝纤维、氧化锆纤维、岩棉、玄武岩纤维、云母纤维中的一种或者几种。
4.根据权利要求1所述的超薄耐1000℃绝热绝缘柔性无纺布的制备方法，其特征在于，所述耐高温纤维的直径不小于4μm，其长度不小于1mm。
5.根据权利要求1所述的超薄耐1000℃绝热绝缘柔性无纺布的制备方法，其特征在于，S3)中施胶工艺为浸渍法、喷淋法、真空吸胶法、平板式浸轧法、凹版转移涂胶法、圆网转移涂胶法的一种。
6.根据权利要求1所述的超薄耐1000℃绝热绝缘柔性无纺布的制备方法，其特征在于，所述绝热粉末为氧化铝、二氧化硅、氧化钼、二氧化钼、氧化铁、氧化锆、碳化硅、硅酸铝、氧化钛气凝胶粉末中的一种或者几种。
7.根据权利要求1所述的超薄耐1000℃绝热绝缘柔性无纺布的制备方法，其特征在于，所述醇类溶剂为甲醇、乙醇、乙二醇、丙醇、正丁醇、异丁醇、正戊醇、异戊醇、正己醇、异己醇中的一种或几种。
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