CN113980419A - 一种低温降温消融阻隔材料的制备方法 - Google Patents
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Abstract
本发明公开了一种低温降温消融阻隔材料的制备方法，该方法制备的低温降温消融阻隔材料满足在低于350℃时，一方面需要对器件进行阻隔降温保护，同时在器件启用时阻隔件不具有力学阻挡的需求。本发明的低温降温消融阻隔材料的制备方法，其包括以下步骤：将低温解聚材料与基体树脂复合，或将低温解聚材料、低温分解填料与基体树脂复合，得到降温消融阻隔材料，使其能够在低于350℃下进行解聚分解，实现阻隔材料的吸热降温和消融的功能，降温消融阻隔材料的固化成型温度低于60℃。
Description
技术领域
本发明涉及一种复合材料的制备方法，更具体地说涉及一种低温降温消融阻隔材料的制备方法。
背景技术
对于表面温度可达3000～4000℃阻隔环境，需要利用表面材料在热流作用下能发生分解、熔化、蒸发、升华、侵蚀等物理和化学变化，借助材料表面的质量消耗带走大量的热，以达到阻止热流传入。然而在一些低于350℃，一方面需要对器件进行阻隔降温保护，同时在器件启用时阻隔件不能有力学阻挡的应用环境下，高温烧蚀材料已不适，需要开发出一种相对于高温烧蚀材料的低温降温消融阻隔材料的制备方法。
发明内容
本发明的目的是解决现有技术中存在的问题与不足，提供一种低温降温消融阻隔材料的制备方法，该方法制备的低温降温消融阻隔材料满足在低于350℃时，一方面需要对器件进行阻隔降温保护，同时在器件启用时阻隔件不具有力学阻挡的需求。
本发明是通过以下技术方案实现的：
本发明的低温降温消融阻隔材料的制备方法，其包括以下步骤：
将低温解聚材料与基体树脂复合，或将低温解聚材料、低温分解填料与基体树脂复合，得到降温消融阻隔材料，使其能够在低于350℃下进行解聚分解，实现阻隔材料的吸热降温和消融的功能，降温消融阻隔材料的固化成型温度低于60℃。
本发明上述的低温降温消融阻隔材料的制备方法，其进一步的技术方案是所述的复合是将低温解聚材料与基体树脂或低温解聚材料、低温分解填料与基体树脂在密炼机中均匀分散，再加入基体树脂固化剂和基体树脂降解促进剂，压制成型并固化。
本发明上述的低温降温消融阻隔材料的制备方法，其进一步的技术方案还可以是所述的低温解聚材料为分子量分布在1000-3000、平均粒径为20～50um的表面羟基被封端的多聚甲醛粉末；所述的低温分解填料为聚磷酸胺、偶氮二甲基酰胺、偶氮二异丁腈和4,4'-氧代双苯磺酰肼中的一种或其组合；所述的基体树脂降解促进剂为纳米氧化锌、纳米二氧化钛、纳米氧化镧、纳米铈、纳米氧化锑、醋酸镧、醋酸铈、醋酸锑、醋酸锌中的一种或其组合；所述的基体树脂为低于60℃固化的环氧树脂或聚氨酯。再进一步的技术方案是所述的表面羟基被封端的多聚甲醛粉末的处理方法为：将异氰酸溶于石油醚溶剂中，然后将多聚甲醛粉末与异氰酸溶液按质量比100：100～50混合，在常温下密闭反应2h以上，去除石油醚溶剂，获得表面羟基被封端的多聚甲醛。更进一步的技术方案是所述的异氰酸为TDI、HDI或XDI；所述的异氰酸与石油醚的质量比为2～5:100。
本发明上述的低温降温消融阻隔材料的制备方法，其进一步的技术方案还可以是所述的基体树脂用量为20-50份，低温解聚材料用量为30-80份，低温分解填料用量为5-20份。
本发明上述的低温降温消融阻隔材料的制备方法，其进一步的技术方案还可以是所述的基体树脂降解促进剂用量为基体树脂与固化剂总质量的1～3％。
本发明上述的低温降温消融阻隔材料的制备方法，其进一步的技术方案还可以是所述的在密炼机中室温下均匀分散时间5分钟以上，搅拌速度大于60rpm；所述的基体树脂固化剂为环氧树脂固化剂或聚氨酯固化剂。再进一步的技术方案是所述的环氧树脂固化剂为有机叔胺；所述的聚氨酯固化剂为异氰酸。
本发明与现有技术相比具有以下有益效果：
本发明的低温降温消融阻隔材料能够在低于350℃下进行解聚消融，通过解聚吸热实现材料降温；同时通过解聚分解，使阻隔件不具有力学阻挡功能。
附图说明
图1为实施例5制备的低温降温消融阻隔材料吸热消融曲线图
具体实施方式
实施例1
表面羟基被封端的多聚甲醛制备：将5份的TDI溶于100份的石油醚溶剂中，然后将100份的多聚甲醛分散在所获的溶液中，在常温下密闭反应5小时，去除石油醚溶剂，获得表面羟基被封端的多聚甲醛。
实施例2
将80份表面羟基被封端的多聚甲醛与40份E51环氧树脂在密炼机中进行常温均匀分散5min，再加入5份593胺类固化剂分散2分钟，常温压制成型，并在40℃下恒温2h固化，得到低温降温消融阻隔材料。
实施例3
将60份表面羟基被封端的多聚甲醛、10份聚磷酸胺和10份偶氮二甲基酰胺与22份聚醚多元醇在密炼机中进行常温均匀分散5min，再加入8份TDI和0.6份的纳米氧化锌分散2分钟，常温压制成型，并在常温下固化，得到低温降温消融阻隔材料。
实施例4
将40份表面羟基被封端的多聚甲醛、15份聚磷酸胺和5份偶氮二异丁腈与20份聚醚多元醇在密炼机中进行常温均匀分散5min，再加入10份HDI和0.3份的纳米二氧化钛分散5分钟，常温压制成型，并在常温下固化，得到低温降温消融阻隔材料。
实施例5
将60份表面羟基被封端的多聚甲醛与30份聚醚多元醇在密炼机中进行常温均匀分散5min，再加入10份HDI和0.3份的醋酸铈分散5分钟，常温压制成型，并在常温下固化，得到低温降温消融阻隔材料。
Claims (9)
1.一种低温降温消融阻隔材料的制备方法，其特征在于包括以下步骤：
将低温解聚材料与基体树脂复合，或将低温解聚材料、低温分解填料与基体树脂复合，得到降温消融阻隔材料，使其能够在低于350℃下进行解聚分解，实现阻隔材料的吸热降温和消融的功能，降温消融阻隔材料的固化成型温度低于60℃。
2.根据权利要求1所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的复合是将低温解聚材料与基体树脂或低温解聚材料、低温分解填料与基体树脂在密炼机中均匀分散，再加入基体树脂固化剂和基体树脂降解促进剂，压制成型并固化。
3.根据权利要求1或2所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的低温解聚材料为分子量分布在1000-3000、平均粒径为20～50um的表面羟基被封端的多聚甲醛粉末；所述的低温分解填料为聚磷酸胺、偶氮二甲基酰胺、偶氮二异丁腈和4,4'-氧代双苯磺酰肼中的一种或其组合；所述的基体树脂降解促进剂为纳米氧化锌、纳米二氧化钛、纳米氧化镧、纳米铈、纳米氧化锑、醋酸镧、醋酸铈、醋酸锑、醋酸锌中的一种或其组合；所述的基体树脂为低于60℃固化的环氧树脂或聚氨酯。
4.根据权利要求3所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的表面羟基被封端的多聚甲醛粉末的处理方法为：将异氰酸溶于石油醚溶剂中，然后将多聚甲醛粉末与异氰酸溶液按质量比100：100～50混合，在常温下密闭反应2h以上，去除石油醚溶剂，获得表面羟基被封端的多聚甲醛。
5.根据权利要求4所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的异氰酸为TDI、HDI或XDI；所述的异氰酸与石油醚的质量比为2～5:100。
6.根据权利要求3所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的基体树脂用量为20-50份，低温解聚材料用量为30-80份，低温分解填料用量为5-20份。
7.根据权利要求3所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的基体树脂降解促进剂用量为基体树脂与固化剂总质量的1～3％。
8.根据权利要求2所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的在密炼机中室温下均匀分散时间5分钟以上，搅拌速度大于60rpm；所述的基体树脂固化剂为环氧树脂固化剂或聚氨酯固化剂。
9.根据权利要求8所述的低温降温消融阻隔材料的制备方法，其特征在于，所述的环氧树脂固化剂为有机叔胺；所述的聚氨酯固化剂为异氰酸。
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