CN111409208A - 一种耐烧蚀、低导热复合结构绝热层及其制备方法 - Google Patents

一种耐烧蚀、低导热复合结构绝热层及其制备方法 Download PDF

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CN111409208A
CN111409208A CN202010348330.5A CN202010348330A CN111409208A CN 111409208 A CN111409208 A CN 111409208A CN 202010348330 A CN202010348330 A CN 202010348330A CN 111409208 A CN111409208 A CN 111409208A
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parts
heat
ablation
insulating layer
insulation layer
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CN111409208B (zh
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闫宁
栾涛
边城
李宏岩
关轶文
时艺娟
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Xian Modern Chemistry Research Institute
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Abstract

本发明提出一种耐烧蚀、低导热复合结构绝热层及其制备方法，通过有机纤维/无机纤维复配，结合耐高温树脂、补强剂和硅烷偶联剂等组分配比的调控，制备的复合结构绝热层的耐烧蚀性能、拉伸强度和断裂伸长率相比于现有技术显著提高；通过原位发泡技术获得多孔橡胶隔热材料，与现有通过添加空心微球的技术相比，材料导热系数降低更为显著；采用模压工艺实现层状复合结构绝热层成型，在诱导发泡的同时完成耐烧蚀层和隔热层固化交联，获得界面粘接强度可靠的层状复合结构绝热层。本发明的绝热层兼备耐烧蚀和隔热功能，材料制造工艺方法容易实施且稳定可靠，适用于对耐烧蚀和隔热性能同时具有较高要求的固体火箭发动机热防护技术领域。

Description

一种耐烧蚀、低导热复合结构绝热层及其制备方法
技术领域
本发明属于高分子复合材料制备技术领域，具体涉及一种耐烧蚀、低导热复合结构绝热层及其制备方法。
背景技术
新一代远程、高速冲压发动机是武器装备实现快速、远程打击的迫切要求。随着发动机飞行马赫数和射程的增加，燃烧室的工作环境异常恶劣，因此对高性能热防护材料提出了迫切需求。发动机燃烧室热防护材料通常采用橡胶基复合材料。目前，采用单一均质的硅橡胶绝热层已经满足补燃室耐烧蚀和抗粒子冲刷要求，然而，由于材料隔热性能不理想，导致发动机壳体温度过高，显著影响壳体表面电子元器件的正常工作。温升过高甚至严重危及到发动机结构的完整性。为了改善隔热性能，通常需要增加绝热层厚度。然而，高速冲压发动机狭小的隔热空间要求橡胶绝热层必须在有限的厚度内将壳体温度降至安全范围。另外，材料厚度的增加会导致发动机消极重量增加，装药受限，严重影响武器装备的能量和射程。由此可见，单一结构绝热层已经无法满足冲压发动机的热防护需求，迫切需要发展多功能一体化热防护材料。
发明内容
(一)要解决的技术问题
本发明提出一种耐烧蚀、低导热复合结构绝热层及其制备方法，以解决如何提高层状材料界面粘接可靠性，满足复杂工况下发动机的热防护需求的技术问题。
(二)技术方案
为了解决上述技术问题，本发明提出一种耐烧蚀、低导热复合结构绝热层，该复合结构绝热层为由耐烧蚀层和隔热层通过复合模压制备的层状复合结构绝热层；其中，
耐烧蚀层按照重量份包括以下组分：三元乙丙橡胶80-95份，氯磺化聚乙烯5-20份，有机纤维1-5份，无机纤维1-10份，硼酚醛树脂5-20份，二氧化硅5-20份，促进剂1-3份，硫化剂1-2份，硬脂酸1-3份，氧化锌3-5份，增塑剂1-5份，硅烷偶联剂1-5份；
隔热层按照重量份包括以下组分：三元乙丙橡胶80-95份，氯磺化聚乙烯5-20份，硼酚醛树脂5-20份，氧化锌3-5份，硬脂酸1-3份，促进剂1-3份，硫化剂1-2份、发泡剂1-10份。
进一步地，有机纤维为聚对苯二甲酰对苯二胺纤维、聚丙烯腈纤维、聚对苯撑苯并双噁唑纤维中的一种或复合物。
进一步地，无机纤维为高硅氧纤维、碳纤维、莫来石纤维中的一种或复合物。
进一步地，硅烷偶联剂为3-巯丙基三乙氧基硅烷或乙烯基三乙氧基硅烷。
进一步地，增塑剂为癸二酸二异辛酯或石蜡油。
进一步地，促进剂为噻唑类或胍类促进剂。
进一步地，发泡剂为4,4-氧代双苯磺酰肼、偶氮二甲酰胺、二亚硝基五亚甲基四胺中的一种或复合物。
此外，本发明还提出一种耐烧蚀、低导热复合结构绝热层制备方法，该复合结构绝热层制备方法包括如下步骤：
S1、耐烧蚀层生胶片制备：将三元乙丙橡胶和氯磺化聚乙烯在开炼机上混合均匀，出现堆积胶；调整辊距至0.2mm，加入有机纤维，薄通3次；调整辊距至2mm，依次加入氧化锌、硬脂酸、硼酚醛树脂，切胶翻转混合2min；保持辊距不变，依次加入二氧化硅、硅烷偶联剂和增塑剂，混炼3min；加入无机纤维，切胶翻转混炼2min，调整辊距至0.5mm，薄通3次；加入促进剂和硫化剂，混炼2min；调整辊距至2-8mm，出片，冷却放置24h；
S2、隔热层生胶片制备：将三元乙丙橡胶和氯磺化聚乙烯在开炼机上混合均匀，出现堆积胶；依次加入氧化锌、硬脂酸、硼酚醛树脂，切胶翻转混合2min；；加入促进剂，切胶翻转混炼均匀；加入发泡剂，混炼均匀；加入硫化剂，将胶料混炼均匀，调整辊距至0.5mm，薄通5次下料；调整辊距至2-8mm，出片，冷却放置24h；
S3、耐烧蚀、隔热一体化模压复合成型：将耐烧蚀层生胶片与隔热层生胶片剪裁后分别铺贴在厚度可调的模具中；将耐烧蚀层生胶片与隔热层生胶片表面贴合，通过平板硫化机加压，对耐烧蚀层生胶片和隔热层生胶片进行固化处理，然后保压自然降至室温。
进一步地，在步骤S3中，固化压力0.5-10MPa，固化温度130-165℃，保温0.5-2h。
(三)有益效果
本发明提出一种耐烧蚀、低导热复合结构绝热层及其制备方法，通过有机纤维/无机纤维复配，结合耐高温树脂、二氧化硅补强剂和硅烷偶联剂等组分配比的调控，制备的复合结构绝热层的耐烧蚀性能、拉伸强度和断裂伸长率相比于现有技术显著提高；通过原位发泡技术获得多孔橡胶隔热材料，与现有通过添加空心微球的技术相比，材料导热系数降低更为显著；采用模压工艺实现层状复合结构绝热层成型，在诱导发泡的同时完成耐烧蚀层和隔热层固化交联，获得界面粘接强度可靠的层状复合结构绝热层。本发明的绝热层兼备耐烧蚀和隔热功能，材料制造工艺方法容易实施且稳定可靠，适用于对耐烧蚀和隔热性能同时具有较高要求的固体火箭发动机热防护技术领域。
附图说明
图1为本发明实施例的耐烧蚀层/发泡隔热层复合结构绝热层结构示意图；
图2为本发明实施例的耐烧蚀层/空心微球隔热层复合结构绝热层结构示意图。
具体实施方式
为使本发明的目的、内容和优点更加清楚，下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。
实施例
本实施例提出一种耐烧蚀层/发泡隔热层复合结构绝热层及其制备方法，制备方法包括如下步骤：
S1、耐烧蚀层生胶片制备：将三元乙丙橡胶95份和氯磺化聚乙烯5份在开炼机上混合均匀；调整辊距至0.2mm，加入聚对苯二甲酰对苯二胺纤维2.5份，薄通3次；调整辊距至2mm，依次加入氧化锌3份、硬脂酸1份、硼酚醛树脂15份，切胶翻转混合2min；保持辊距不变，依次加入二氧化硅20份，硅烷偶联剂1份，石蜡油5份，混炼3min；加入碳纤维3份，切胶翻转混炼2min，调整辊距至0.5mm，薄通3次；加入噻唑类促进剂3份，硫化剂1份，混炼2min；调整辊距至5mm，出片，冷却放置24h；
S2、隔热层生胶片制备：将三元乙丙橡胶95份和氯磺化聚乙烯5份在开炼机上混合均匀，出现适量堆积胶；依次加入氧化锌3份、硬脂酸1份、硼酚醛树脂20份，切胶翻转混合2min；保持辊距不变，依次加入二氧化硅20份，KH-580硅烷偶联剂1份，石蜡油5份，混炼3min；加入噻唑类促进剂3份，切胶翻转混炼均匀；然后，加入偶氮二甲酰胺发泡剂(AC)5份，切胶翻转混炼均匀；加入硫化剂1.5份，将胶料混炼均匀，调整辊距至0.5mm，薄通5次下料；调整辊距至3mm，出片，冷却放置24h。
S3、耐烧蚀、隔热一体化模压复合成型：将厚度5mm的耐烧蚀层生胶片与厚度3mm的隔热层生胶片剪裁合适的尺寸，分别铺贴在厚度可调的模具中；将耐烧蚀层生胶片与隔热层生胶片表面贴合，通过平板硫化机加压，对耐烧蚀层生胶片和隔热层生胶片进行固化处理，固化压力2MPa，在165℃保温2h，然后保压自然降至室温。获得的如图1所示的双层复合结构绝热层，绝热层线烧蚀率为0.06mm·s-1，导热系数为0.08W·m-1K-1。
对比实施例
S1、耐烧蚀层生胶片制备：将三元乙丙橡胶95份和氯磺化聚乙烯5份在开炼机上混合均匀；调整辊距至0.2mm，加入聚对苯二甲酰对苯二胺纤维2.5份，薄通3次；调整辊距至2mm，依次加入氧化锌3份、硬脂酸1份、硼酚醛树脂15份，切胶翻转混合2min；保持辊距不变，依次加入二氧化硅20份，KH-580硅烷偶联剂1份，石蜡油5份，混炼3min；加入噻唑类促进剂3份，硫化剂1份，混炼2min；调整辊距至5mm，出片，冷却放置24h；
S2、隔热层生胶片制备：将三元乙丙橡胶95份和氯磺化聚乙烯5份在开炼机上混合均匀，出现适量堆积胶；依次加入氧化锌3份、硬脂酸1份、硼酚醛树脂20份，切胶翻转混合2min；依次加入二氧化硅20份，KH-580硅烷偶联剂1份，石蜡油5份，混炼3min；加入噻唑类促进剂3份，空心玻璃微球5份，切胶翻转混炼均匀；加入硫化剂1.5份，将胶料混炼均匀，调整辊距至0.5mm，薄通5次下料；调整辊距至3mm，出片，冷却放置24h；
S3、耐烧蚀、隔热一体化模压复合成型：将厚度5mm的耐烧蚀层生胶片与厚度3mm的隔热层生胶片剪裁合适的尺寸，分别铺贴在厚度可调的模具中；将耐烧蚀层生胶片与隔热层生胶片表面贴合，通过平板硫化机加压，对耐烧蚀层生胶片和隔热层生胶片进行固化处理，固化压力为2MPa，在165℃保温2h，然后保压自然降至室温。获得如图2所示的双层复合结构绝热层，绝热层线烧蚀率为0.15mm·s-1，导热系数为0.24W·m-1K-1。
由上述实施例和对比实施例可以看出，本发明采用有机纤维/无机纤维复配可以显著提高绝热层的耐烧蚀性能；同时，与添加空心微球相比，采用发泡工艺制备的隔热层的导热系数显著降低。这是因为，空心微球在橡胶加工过程中容易破碎，从而显著降低微球隔热效能；通过原位热压发泡工艺制备泡孔尺寸分布均匀的结构，工艺稳定，更有利于降低材料的导热系数。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变形，这些改进和变形也应视为本发明的保护范围。

Claims (9)

1.一种耐烧蚀、低导热复合结构绝热层，其特征在于，所述复合结构绝热层为由耐烧蚀层和隔热层通过复合模压制备的层状复合结构绝热层；其中，
所述耐烧蚀层按照重量份包括以下组分：三元乙丙橡胶80-95份，氯磺化聚乙烯5-20份，有机纤维1-5份，无机纤维1-10份，硼酚醛树脂5-20份，二氧化硅5-20份，促进剂1-3份，硫化剂1-2份，硬脂酸1-3份，氧化锌3-5份，增塑剂1-5份，硅烷偶联剂1-5份；
所述隔热层按照重量份包括以下组分：三元乙丙橡胶80-95份，氯磺化聚乙烯5-20份，硼酚醛树脂5-20份，氧化锌3-5份，硬脂酸1-3份，促进剂1-3份，硫化剂1-2份、发泡剂1-10份。
2.如权利要求1所述的复合结构绝热层，其特征在于，所述有机纤维为聚对苯二甲酰对苯二胺纤维、聚丙烯腈纤维、聚对苯撑苯并双噁唑纤维中的一种或复合物。
3.如权利要求1所述的复合结构绝热层，其特征在于，所述无机纤维为高硅氧纤维、碳纤维、莫来石纤维中的一种或复合物。
4.如权利要求1所述的复合结构绝热层，其特征在于，所述硅烷偶联剂为3-巯丙基三乙氧基硅烷或乙烯基三乙氧基硅烷。
5.如权利要求1所述的复合结构绝热层，其特征在于，所述增塑剂为癸二酸二异辛酯或石蜡油。
6.如权利要求1所述的复合结构绝热层，其特征在于，所述促进剂为噻唑类或胍类促进剂。
7.如权利要求1所述的复合结构绝热层，其特征在于，所述发泡剂为4,4-氧代双苯磺酰肼、偶氮二甲酰胺、二亚硝基五亚甲基四胺中的一种或复合物。
8.一种耐烧蚀、低导热复合结构绝热层制备方法，其特征在于，所述复合结构绝热层制备方法包括如下步骤：
S1、耐烧蚀层生胶片制备：将三元乙丙橡胶和氯磺化聚乙烯在开炼机上混合均匀，出现堆积胶；调整辊距至0.2mm，加入有机纤维，薄通3次；调整辊距至2mm，依次加入氧化锌、硬脂酸、硼酚醛树脂，切胶翻转混合2min；保持辊距不变，依次加入二氧化硅、硅烷偶联剂和增塑剂，混炼3min；加入无机纤维，切胶翻转混炼2min，调整辊距至0.5mm，薄通3次；加入促进剂和硫化剂，混炼2min；调整辊距至2-8mm，出片，冷却放置24h；
S2、隔热层生胶片制备：将三元乙丙橡胶和氯磺化聚乙烯在开炼机上混合均匀，出现堆积胶；依次加入氧化锌、硬脂酸、硼酚醛树脂，切胶翻转混合2min；加入促进剂，切胶翻转混炼均匀；加入发泡剂，混炼均匀；加入硫化剂，将胶料混炼均匀，调整辊距至0.5mm，薄通5次下料；调整辊距至2-8mm，出片，冷却放置24h；
S3、耐烧蚀、隔热一体化模压复合成型：将耐烧蚀层生胶片与隔热层生胶片剪裁后分别铺贴在厚度可调的模具中；将耐烧蚀层生胶片与隔热层生胶片表面贴合，通过平板硫化机加压，对耐烧蚀层生胶片和隔热层生胶片进行固化处理，然后保压自然降至室温。
9.如权利要求8所述的复合结构绝热层制备方法，其特征在于，在步骤S3中，固化压力0.5-10MPa，固化温度130-165℃，保温0.5-2h。
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