CN111746063A - 一种轻质隔热阻燃弹性面料及其制备方法 - Google Patents

一种轻质隔热阻燃弹性面料及其制备方法 Download PDF

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Publication number
CN111746063A
CN111746063A CN202010636167.2A CN202010636167A CN111746063A CN 111746063 A CN111746063 A CN 111746063A CN 202010636167 A CN202010636167 A CN 202010636167A CN 111746063 A CN111746063 A CN 111746063A
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flame
retardant
stirring
layer
outer layer
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张为凤
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Nantong Weixing Textile Technology Co ltd
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Nantong Weixing Textile Technology Co ltd
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Laminated Bodies (AREA)

Abstract

本发明公开了一种轻质隔热阻燃弹性面料及其制备方法，其中包括基布、阻燃内层和防火外层，基布由聚苯并咪唑纤维编织得到，其中聚苯并咪唑纤维的阻燃性较好，在空气中完全不燃烧，热稳定性和耐化学试剂性也非常优异；所述基布、阻燃内层之间、阻燃内层和防火外层之间均设置有粘结层；在操作时，粘结层包括但不仅限于磷酸铝粘结剂，其他任何具有粘结性能的材料也能作为粘结层，该粘结层可用于基层、阻燃内层和防火外层之间的粘结；本发明工艺设计合理，操作简单，制备得到的面料具有优异的阻燃性能和隔热性能，且该面料同样具有优异的高温稳定性，可适用于消防等高温防火环境下，应用范围广泛，具有较高的实用性。

Description

一种轻质隔热阻燃弹性面料及其制备方法
技术领域
本发明涉及面料加工技术领域，具体是一种轻质隔热阻燃弹性面料及其制备方法。
背景技术
阻燃面料，一种可以延缓火焰燃烧的特种织物，阻燃面料又分为后整理阻燃和原料纱线阻燃；现如今，随着科技的进步和现代工业的发展，具有优异隔热阻燃性能的新材料不断地被开发，也在不断的引起我们的关注。
常规阻燃面料为多层级布料复合制备，在高温下，由于面料各层之间的热膨胀特异性不一致，面料层级之间容易出现间隙，这种情况不仅容易导致面料变形，而且间隙的存在也会影响布料整体的隔热性能，实际应用带来不便。
针对上述问题，我们公开了一种轻质隔热阻燃弹性面料及其制备方法，以解决该问题。
发明内容
本发明的目的在于提供一种轻质隔热阻燃弹性面料及其制备方法，以解决现有技术中的问题。
为实现上述目的，本发明提供如下技术方案：
一种轻质隔热阻燃弹性面料，所述弹性面料包括基布、阻燃内层和防火外层，所述基布、阻燃内层之间、阻燃内层和防火外层之间均设置有粘结层。
较优化的方案，所述粘结层为磷酸铝粘结剂，所述基布由聚苯并咪唑纤维编织得到。
较优化的方案，所述阻燃内层各组分原料包括，以重量计，改性二氧化硅凝胶10-20份、改性聚酰胺纤维8-12份、氧化铝纤维3-5份、可膨胀石墨18-25份。
较优化的方案，所述改性聚酰胺纤维主要由聚酰胺纤维、高锰酸钾、浓硫酸、丙烯酸制备得到。
较优化的方案，所述改性二氧化硅凝胶主要由二氧化硅凝胶、环氧氯丙烷、高氯酸、无水乙醇制备得到。
较优化的方案，所述防火外层主要由预处理外层、聚乙二醇、环氧树脂、过硫酸钾、二氧化钛、中空微球制备得到。
较优化的方案，所述预处理外层包括亚麻纤维、玄武岩纤维和芳纶纤维，所述亚麻纤维、玄武岩纤维和芳纶纤维的质量比为1：(2-3)：1。
较优化的方案，所述可膨胀石墨粒径为0.15-0.3mm，所述氧化铝纤维为短切纤维，直径为2-8μm，长度2-4mm。
较优化的方案，一种轻质隔热阻燃弹性面料的制备方法，包括以下步骤：
1)防火外层的制备；
A.取亚麻纤维、玄武岩纤维和芳纶纤维，混合纺丝，再织成布料，水洗烘干，定型，得到预处理外层；
B.取聚乙二醇、环氧树脂，混合搅拌，再置于65-68℃下水浴中，搅拌，接着缓慢加入过硫酸钾，混合均匀后置于180-185℃油浴中，搅拌反应，得到物料A；
C.取物料A，加入环氧树脂，再置于65-68℃下水浴中，搅拌剪切50-60min，接着加入二氧化钛和中空微球，继续搅拌，依次加入消泡剂、分散剂和固化剂，搅拌均匀后加入预处理外层，浸渍，得到防火外层；
2)阻燃内层的制备；
a)取聚酰胺纤维，置于甲酸溶液中浸泡，水洗烘干，再置于去离子水中，加热至65-68℃，氮气环境下加入高锰酸钾和浓硫酸，缓慢降温至60-62℃，再加入丙烯酸，反应，得到改性聚酰胺纤维；
b)取改性聚酰胺纤维、氧化铝纤维，置于去离子水中，超声分散，再加入可膨胀石墨，真空抽滤成型，得到预处理阻燃内层；
c)取聚磷酸铵、氢氧化镁、氢氧化铝和无水乙醇，搅拌混合，超声分散，得到物料B；取正硅酸四乙酯和无水乙醇，混合搅拌，再加入物料B，搅拌，接着加入盐酸，搅拌，静置，洗涤，得到二氧化硅凝胶；
d)取环氧氯丙烷、高氯酸和无水乙醇，搅拌，再加入二氧化硅凝胶，静置，无水乙醇洗涤，再加入乙二胺无水乙醇混合溶液，保温处理，再加入预处理阻燃内层，浸泡，得到阻燃内层；
3)取待处理基布，置于聚氨酯树脂中浸泡，浸轧、焙烘，冷却至室温，得到基布；
4)取基布、阻燃内层、防火外层和粘结层，以自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，得到弹性面料。
较优化的方案，包括以下步骤：
1)防火外层的制备；
A.取亚麻纤维、玄武岩纤维和芳纶纤维，混合纺丝，再织成布料，水洗，150-160℃下烘干，定型，得到预处理外层；
B.取聚乙二醇、环氧树脂，混合搅拌5-8min，再置于65-68℃下水浴中，搅拌30-40min，搅拌转速为250-300r/min，接着缓慢加入过硫酸钾，混合均匀后置于180-185℃油浴中，搅拌反应4-5h，得到物料A；
C.取物料A，加入环氧树脂，再置于65-68℃下水浴中，3500r/min转速下搅拌剪切50-60min，接着加入二氧化钛和中空微球，继续搅拌10-12min，依次加入消泡剂、分散剂和固化剂，搅拌均匀后加入预处理外层，浸渍40-50min，得到防火外层；
2)阻燃内层的制备；
a)取聚酰胺纤维，置于甲酸溶液中浸泡20-25min，水洗烘干，再置于去离子水中，加热至65-68℃，氮气环境下加入高锰酸钾和浓硫酸，浸泡10-15min，缓慢降温至60-62℃，再加入丙烯酸，反应4-4.5h，得到改性聚酰胺纤维；
b)取改性聚酰胺纤维、氧化铝纤维，置于去离子水中，超声分散5-10min，再加入可膨胀石墨，真空抽滤成型，得到预处理阻燃内层；
c)取聚磷酸铵、氢氧化镁、氢氧化铝和无水乙醇，搅拌混合15-20min，超声分散1-2h，得到物料B；取正硅酸四乙酯和无水乙醇，混合搅拌5-10min，再加入物料B，25℃下搅拌10-12h，接着加入盐酸，搅拌15-18min，静置10-12h，去离子水、无水乙醇交换洗涤2-3次，得到二氧化硅凝胶；
d)取环氧氯丙烷、高氯酸和无水乙醇，搅拌5-8min，再加入二氧化硅凝胶，25-28℃下静置10-12h，无水乙醇洗涤，再加入乙二胺无水乙醇混合溶液，置于50-55℃水浴下保温处理12-14h，再加入预处理阻燃内层，在35-40℃下浸泡2-3h，得到阻燃内层；
3)取待处理基布，置于聚氨酯树脂中浸泡5-10min，浸轧、焙烘，冷却至室温，得到基布；
4)取基布、阻燃内层、防火外层和粘结层，以自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，成型温度为120-125℃，成型时间为12-14h，得到弹性面料。
与现有技术相比，本发明的有益效果是：
本申请公开了一种轻质隔热阻燃弹性面料及其制备方法，其中包括基布、阻燃内层和防火外层，基布由聚苯并咪唑纤维编织得到，其中聚苯并咪唑纤维的阻燃性较好，在空气中完全不燃烧，热稳定性和耐化学试剂性也非常优异；所述基布、阻燃内层之间、阻燃内层和防火外层之间均设置有粘结层；在操作时，粘结层包括但不仅限于磷酸铝粘结剂，其他任何具有粘结性能的材料也能作为粘结层，该粘结层可用于基层、阻燃内层和防火外层之间的粘结。
在制备时，本申请先进行防火外层的制备，由于玄武岩纤维的阻燃性能较优异，其热系数为0.031W/m·K-0.038W/m·K，隔热性能也十分优异；芳纶纤维具有永久阻燃性，在高温条件下也十分稳定，不会发生熔融；基于上述特性，本申请防火外层采用亚麻纤维、玄武岩纤维和芳纶纤维混纺编织，烘干定型后得到预处理外层，该预处理外层具有优异的隔热、阻燃性能；接着本申请利用水性环氧树脂作为成膜物质，加入隔热降温的中空微珠、消泡剂、分散剂和固化剂等物料，制备得到具有热反射性能的物料，将预处理外层置于物料中浸渍，制备得到防火外层，该防火外层不仅具有优异的阻燃、隔热性能，而且热反射性能优异，可进一步协调提高产品的隔热性能；水性环氧树脂的存在使得防火外层和阻燃内层的粘结性能更加优异，面料层级之间附着力更高。
本发明还制备了一种阻燃内层，在制备时先利用聚酰胺纤维、高锰酸钾和浓硫酸进行反应，在聚酰胺纤维表面接枝共聚丙烯，其中高锰酸钾和浓硫酸作为氧化还原体系，制备得到的改性聚酰胺纤维表面含有活性较强的羧基基团；接着本发明又利用改性聚酰胺纤维、氧化铝纤维和可膨胀石墨，真空抽滤成型，得到预处理阻燃内层，该预处理阻燃内层中以改性聚酰胺纤维、氧化铝纤维为基体材料，可保证阻燃内层的阻燃性能，同时以可膨胀石墨为膨胀源，可膨胀石墨在高温环境中其层间化合物会快速分解、汽化，释放的气体生的推力使石墨层间剥离，形成体积膨胀，这样不仅能够提高面料的力学性能，且能够避免高温下面料各层级因为热膨胀性能不同，从而出现空隙导致隔热性能下降的问题。
本发明中还制备了利用聚磷酸铵、氢氧化镁、氢氧化铝作为原料，制备得到阻燃性能优异的二氧化硅凝胶，随即通过环氧氯丙烷、高氯酸和无水乙醇对其进行氨基化改性，制备得到氨基接枝改性的改性二氧化硅凝胶，预处理阻燃内层置于改性二氧化硅凝胶中浸泡时，预处理阻燃内层表明的羟基会与氨基相互结合，使得预处理阻燃内层表面包覆一层改性二氧化硅凝胶，提高改性二氧化硅凝胶附着力的同时进一步提高产品的阻燃性能；最后本申请利用待处理基布在聚氨酯树脂中浸泡，在依据自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，得到具有优异阻燃、隔热、防火性能的面料成品。
本发明公开了一种轻质隔热阻燃弹性面料及其制备方法，工艺设计合理，操作简单，制备得到的面料具有优异的阻燃性能和隔热性能，且该面料同样具有优异的高温稳定性，可适用于消防等高温防火环境下，应用范围广泛，具有较高的实用性。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1：
S1：防火外层的制备；
取亚麻纤维、玄武岩纤维和芳纶纤维，混合纺丝，再织成布料，水洗，150℃下烘干，定型，得到预处理外层；
取聚乙二醇、环氧树脂，混合搅拌5min，再置于65℃下水浴中，搅拌30min，搅拌转速为250r/min，接着缓慢加入过硫酸钾，混合均匀后置于180℃油浴中，搅拌反应4h，得到物料A；
取物料A，加入环氧树脂，再置于65℃下水浴中，3500r/min转速下搅拌剪切50min，接着加入二氧化钛和中空微球，继续搅拌10min，依次加入消泡剂、分散剂和固化剂，搅拌均匀后加入预处理外层，浸渍40min，得到防火外层；
S2：阻燃内层的制备；
取聚酰胺纤维，置于甲酸溶液中浸泡20min，水洗烘干，再置于去离子水中，加热至65℃，氮气环境下加入高锰酸钾和浓硫酸，浸泡10min，缓慢降温至60℃，再加入丙烯酸，反应4-h，得到改性聚酰胺纤维；
取改性聚酰胺纤维、氧化铝纤维，置于去离子水中，超声分散5min，再加入可膨胀石墨，真空抽滤成型，得到预处理阻燃内层；
取聚磷酸铵、氢氧化镁、氢氧化铝和无水乙醇，搅拌混合15min，超声分散1h，得到物料B；取正硅酸四乙酯和无水乙醇，混合搅拌5min，再加入物料B，25℃下搅拌10h，接着加入盐酸，搅拌15min，静置10h，去离子水、无水乙醇交换洗涤2次，得到二氧化硅凝胶；
取环氧氯丙烷、高氯酸和无水乙醇，搅拌5min，再加入二氧化硅凝胶，25℃下静置10h，无水乙醇洗涤，再加入乙二胺无水乙醇混合溶液，置于50℃水浴下保温处理12h，再加入预处理阻燃内层，在35℃下浸泡2-3h，得到阻燃内层；
S3：取待处理基布，置于聚氨酯树脂中浸泡5min，浸轧、焙烘，冷却至室温，得到基布；
取基布、阻燃内层、防火外层和粘结层，以自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，成型温度为120℃，成型时间为12h，得到弹性面料。
本实施例中，所述弹性面料包括基布、阻燃内层和防火外层，所述基布、阻燃内层之间、阻燃内层和防火外层之间均设置有粘结层；所述粘结层为磷酸铝粘结剂，其中磷酸铝粘结剂制备时，先通过磷酸、氢氧化铝反应制备磷酸二氢铝，接着加入水稀释得到磷酸铝粘结剂；所述基布由聚苯并咪唑纤维编织得到。
其中阻燃内层各组分原料包括，以重量计，改性二氧化硅凝胶10份、改性聚酰胺纤维8份、氧化铝纤维3份、可膨胀石墨18份；预处理外层包括亚麻纤维、玄武岩纤维和芳纶纤维，所述亚麻纤维、玄武岩纤维和芳纶纤维的质量比为1：2：1；可膨胀石墨粒径为0.15mm，所述氧化铝纤维为短切纤维，直径为2μm，长度2mm。
实施例2：
S1：防火外层的制备；
取亚麻纤维、玄武岩纤维和芳纶纤维，混合纺丝，再织成布料，水洗，155℃下烘干，定型，得到预处理外层；
取聚乙二醇、环氧树脂，混合搅拌7min，再置于67℃下水浴中，搅拌35min，搅拌转速为280r/min，接着缓慢加入过硫酸钾，混合均匀后置于182℃油浴中，搅拌反应4.5h，得到物料A；
取物料A，加入环氧树脂，再置于66℃下水浴中，3500r/min转速下搅拌剪切55min，接着加入二氧化钛和中空微球，继续搅拌11min，依次加入消泡剂、分散剂和固化剂，搅拌均匀后加入预处理外层，浸渍45min，得到防火外层；
S2：阻燃内层的制备；
取聚酰胺纤维，置于甲酸溶液中浸泡22min，水洗烘干，再置于去离子水中，加热至67℃，氮气环境下加入高锰酸钾和浓硫酸，浸泡12min，缓慢降温至61℃，再加入丙烯酸，反应4.2h，得到改性聚酰胺纤维；
取改性聚酰胺纤维、氧化铝纤维，置于去离子水中，超声分散8min，再加入可膨胀石墨，真空抽滤成型，得到预处理阻燃内层；
取聚磷酸铵、氢氧化镁、氢氧化铝和无水乙醇，搅拌混合18min，超声分散1.5h，得到物料B；取正硅酸四乙酯和无水乙醇，混合搅拌8min，再加入物料B，25℃下搅拌11h，接着加入盐酸，搅拌17min，静置11h，去离子水、无水乙醇交换洗涤2次，得到二氧化硅凝胶；
取环氧氯丙烷、高氯酸和无水乙醇，搅拌7min，再加入二氧化硅凝胶，26℃下静置11h，无水乙醇洗涤，再加入乙二胺无水乙醇混合溶液，置于53℃水浴下保温处理13h，再加入预处理阻燃内层，在39℃下浸泡2.5h，得到阻燃内层；
S3：取待处理基布，置于聚氨酯树脂中浸泡8min，浸轧、焙烘，冷却至室温，得到基布；
取基布、阻燃内层、防火外层和粘结层，以自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，成型温度为123℃，成型时间为13h，得到弹性面料。
本实施例中，所述弹性面料包括基布、阻燃内层和防火外层，所述基布、阻燃内层之间、阻燃内层和防火外层之间均设置有粘结层；所述粘结层为磷酸铝粘结剂，其中磷酸铝粘结剂制备时，先通过磷酸、氢氧化铝反应制备磷酸二氢铝，接着加入水稀释得到磷酸铝粘结剂；所述基布由聚苯并咪唑纤维编织得到。
其中阻燃内层各组分原料包括，以重量计，改性二氧化硅凝胶15份、改性聚酰胺纤维10份、氧化铝纤维4份、可膨胀石墨22份；预处理外层包括亚麻纤维、玄武岩纤维和芳纶纤维，所述亚麻纤维、玄武岩纤维和芳纶纤维的质量比为1：2.5：1；可膨胀石墨粒径为0.22mm，所述氧化铝纤维为短切纤维，直径为6μm，长度3mm。
实施例3：
S1：防火外层的制备；
取亚麻纤维、玄武岩纤维和芳纶纤维，混合纺丝，再织成布料，水洗，160℃下烘干，定型，得到预处理外层；
取聚乙二醇、环氧树脂，混合搅拌8min，再置于68℃下水浴中，搅拌40min，搅拌转速为300r/min，接着缓慢加入过硫酸钾，混合均匀后置于180-185℃油浴中，搅拌反应5h，得到物料A；
取物料A，加入环氧树脂，再置于68℃下水浴中，3500r/min转速下搅拌剪切60min，接着加入二氧化钛和中空微球，继续搅拌12min，依次加入消泡剂、分散剂和固化剂，搅拌均匀后加入预处理外层，浸渍50min，得到防火外层；
S2：阻燃内层的制备；
取聚酰胺纤维，置于甲酸溶液中浸泡25min，水洗烘干，再置于去离子水中，加热至68℃，氮气环境下加入高锰酸钾和浓硫酸，浸泡15min，缓慢降温至62℃，再加入丙烯酸，反应4.5h，得到改性聚酰胺纤维；
取改性聚酰胺纤维、氧化铝纤维，置于去离子水中，超声分散10min，再加入可膨胀石墨，真空抽滤成型，得到预处理阻燃内层；
取聚磷酸铵、氢氧化镁、氢氧化铝和无水乙醇，搅拌混合20min，超声分散2h，得到物料B；取正硅酸四乙酯和无水乙醇，混合搅拌10min，再加入物料B，25℃下搅拌12h，接着加入盐酸，搅拌18min，静置12h，去离子水、无水乙醇交换洗涤3次，得到二氧化硅凝胶；
取环氧氯丙烷、高氯酸和无水乙醇，搅拌8min，再加入二氧化硅凝胶，28℃下静置12h，无水乙醇洗涤，再加入乙二胺无水乙醇混合溶液，置于55℃水浴下保温处理14h，再加入预处理阻燃内层，在40℃下浸泡3h，得到阻燃内层；
S3：取待处理基布，置于聚氨酯树脂中浸泡10min，浸轧、焙烘，冷却至室温，得到基布；
取基布、阻燃内层、防火外层和粘结层，以自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，成型温度为125℃，成型时间为14h，得到弹性面料。
本实施例中，所述弹性面料包括基布、阻燃内层和防火外层，所述基布、阻燃内层之间、阻燃内层和防火外层之间均设置有粘结层；所述粘结层为磷酸铝粘结剂，其中磷酸铝粘结剂制备时，先通过磷酸、氢氧化铝反应制备磷酸二氢铝，接着加入水稀释得到磷酸铝粘结剂；所述基布由聚苯并咪唑纤维编织得到。
其中阻燃内层各组分原料包括，以重量计，改性二氧化硅凝胶20份、改性聚酰胺纤维12份、氧化铝纤维5份、可膨胀石墨25份；预处理外层包括亚麻纤维、玄武岩纤维和芳纶纤维，所述亚麻纤维、玄武岩纤维和芳纶纤维的质量比为1：3：1；可膨胀石墨粒径为0.3mm，所述氧化铝纤维为短切纤维，直径为8μm，长度4mm。
试验：
1、隔热性能检测：
取实施例1-3制备的面料样品，进行防火隔热性能检测，具体检测方法为：
测试时分别在防火外层一侧和基布一侧均放置温度传感器(TM-902C数字温度计)，观察面料样品在450℃高温火焰下燃烧300s，冷热面温度随时间变化情况，记录每隔10s的冷热面温度；其中坐式酒精喷灯位于防火外层一侧。
结论：检测后发现，实施例1-3制备的面料样品在450℃高温火焰下燃烧，其测试两面的温度差在386℃-451℃之间，基布一层温度上升缓慢，且测试过程中基布一层温度系不超过35℃。
由上可知，实施例1-3制备的面料具有优异的隔热性能。
2、热稳定性：
取实施例1-3制备的面料样品，分别沿平行织物经向(或纬向)的方向，试样剪裁尺寸为100mmxl00mm，作为测试样品。
测试前将测试样品置于标准大气条件下调湿平衡24h，再设定温度为260℃，将测试样品置于马弗炉中，关闭阀门，放置5min后取出，检测试样尺寸并计算尺寸变化率。
项目 实施例1 实施例2 实施例3
经向尺寸变化率 0.23％ 0.21％ 0.26％
纬向尺寸变化率 0.32％ 0.28％ 0.29％
结论：实施例1-3制备的测试样品的经向尺寸变化率、纬向尺寸变化率均小于0.5％，试样形态稳定，表面无明显变化，无软化现象；该结果可表明本实施例制备的面料具有优异的热稳定性。
3、阻燃性能：
取实施例1-3制备的面料样品，分别依据本试验参照国标GB/T5455.2014《纺织品燃烧性能标准》进行测试，检测数据如下表所示：
项目 实施例1 实施例2 实施例3
续燃时间 0 0 0
阴燃时间 0.2 0.1 0.2
损毁程度 12.8mm 9.7mm 10.5mm
结论：实施例1-3制备的面料的续燃、阴燃时间均小于2s。。，燃烧时观察发现无熔融、滴落现象，面料损毁度低；该结果可表明本实施例制备的面料具有优异的阻燃性能。
本发明工艺设计合理，操作简单，制备得到的面料具有优异的阻燃性能和隔热性能，且该面料同样具有优异的高温稳定性，可适用于消防等高温防火环境下，应用范围广泛，具有较高的实用性。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。

Claims (10)

1.一种轻质隔热阻燃弹性面料，其特征在于：所述弹性面料包括基布、阻燃内层和防火外层，所述基布、阻燃内层之间、阻燃内层和防火外层之间均设置有粘结层。
2.根据权利要求1所述的一种轻质隔热阻燃弹性面料，其特征在于：所述粘结层为磷酸铝粘结剂，所述基布由聚苯并咪唑纤维编织得到。
3.根据权利要求1所述的一种轻质隔热阻燃弹性面料，其特征在于：所述阻燃内层各组分原料包括，以重量计，改性二氧化硅凝胶10-20份、改性聚酰胺纤维8-12份、氧化铝纤维3-5份、可膨胀石墨18-25份。
4.根据权利要求3所述的一种轻质隔热阻燃弹性面料，其特征在于：所述改性聚酰胺纤维主要由聚酰胺纤维、高锰酸钾、浓硫酸、丙烯酸制备得到。
5.根据权利要求3所述的一种轻质隔热阻燃弹性面料，其特征在于：所述改性二氧化硅凝胶主要由二氧化硅凝胶、环氧氯丙烷、高氯酸、无水乙醇制备得到。
6.根据权利要求1所述的一种轻质隔热阻燃弹性面料，其特征在于：所述防火外层主要由预处理外层、聚乙二醇、环氧树脂、过硫酸钾、二氧化钛、中空微球制备得到。
7.根据权利要求6所述的一种轻质隔热阻燃弹性面料，其特征在于：所述预处理外层包括亚麻纤维、玄武岩纤维和芳纶纤维，所述亚麻纤维、玄武岩纤维和芳纶纤维的质量比为1：(2-3)：1。
8.根据权利要求3所述的一种轻质隔热阻燃弹性面料，其特征在于：所述可膨胀石墨粒径为0.15-0.3mm，所述氧化铝纤维为短切纤维，直径为2-8μm，长度2-4mm。
9.一种轻质隔热阻燃弹性面料的制备方法，其特征在于：包括以下步骤：
1)防火外层的制备；
A.取亚麻纤维、玄武岩纤维和芳纶纤维，混合纺丝，再织成布料，水洗烘干，定型，得到预处理外层；
B.取聚乙二醇、环氧树脂，混合搅拌，再置于65-68℃下水浴中，搅拌，接着缓慢加入过硫酸钾，混合均匀后置于180-185℃油浴中，搅拌反应，得到物料A；
C.取物料A，加入环氧树脂，再置于65-68℃下水浴中，搅拌剪切50-60min，接着加入二氧化钛和中空微球，继续搅拌，依次加入消泡剂、分散剂和固化剂，搅拌均匀后加入预处理外层，浸渍，得到防火外层；
2)阻燃内层的制备；
a)取聚酰胺纤维，置于甲酸溶液中浸泡，水洗烘干，再置于去离子水中，加热至65-68℃，氮气环境下加入高锰酸钾和浓硫酸，缓慢降温至60-62℃，再加入丙烯酸，反应，得到改性聚酰胺纤维；
b)取改性聚酰胺纤维、氧化铝纤维，置于去离子水中，超声分散，再加入可膨胀石墨，真空抽滤成型，得到预处理阻燃内层；
c)取聚磷酸铵、氢氧化镁、氢氧化铝和无水乙醇，搅拌混合，超声分散，得到物料B；取正硅酸四乙酯和无水乙醇，混合搅拌，再加入物料B，搅拌，接着加入盐酸，搅拌，静置，洗涤，得到二氧化硅凝胶；
d)取环氧氯丙烷、高氯酸和无水乙醇，搅拌，再加入二氧化硅凝胶，静置，无水乙醇洗涤，再加入乙二胺无水乙醇混合溶液，保温处理，再加入预处理阻燃内层，浸泡，得到阻燃内层；
3)取待处理基布，置于聚氨酯树脂中浸泡，浸轧、焙烘，冷却至室温，得到基布；
4)取基布、阻燃内层、防火外层和粘结层，以自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，得到弹性面料。
10.根据权利要求9所述的一种轻质隔热阻燃弹性面料的制备方法，其特征在于：包括以下步骤：
1)防火外层的制备；
A.取亚麻纤维、玄武岩纤维和芳纶纤维，混合纺丝，再织成布料，水洗，150-160℃下烘干，定型，得到预处理外层；
B.取聚乙二醇、环氧树脂，混合搅拌5-8min，再置于65-68℃下水浴中，搅拌30-40min，搅拌转速为250-300r/min，接着缓慢加入过硫酸钾，混合均匀后置于180-185℃油浴中，搅拌反应4-5h，得到物料A；
C.取物料A，加入环氧树脂，再置于65-68℃下水浴中，3500r/min转速下搅拌剪切50-60min，接着加入二氧化钛和中空微球，继续搅拌10-12min，依次加入消泡剂、分散剂和固化剂，搅拌均匀后加入预处理外层，浸渍40-50min，得到防火外层；
2)阻燃内层的制备；
a)取聚酰胺纤维，置于甲酸溶液中浸泡20-25min，水洗烘干，再置于去离子水中，加热至65-68℃，氮气环境下加入高锰酸钾和浓硫酸，浸泡10-15min，缓慢降温至60-62℃，再加入丙烯酸，反应4-4.5h，得到改性聚酰胺纤维；
b)取改性聚酰胺纤维、氧化铝纤维，置于去离子水中，超声分散5-10min，再加入可膨胀石墨，真空抽滤成型，得到预处理阻燃内层；
c)取聚磷酸铵、氢氧化镁、氢氧化铝和无水乙醇，搅拌混合15-20min，超声分散1-2h，得到物料B；取正硅酸四乙酯和无水乙醇，混合搅拌5-10min，再加入物料B，25℃下搅拌10-12h，接着加入盐酸，搅拌15-18min，静置10-12h，去离子水、无水乙醇交换洗涤2-3次，得到二氧化硅凝胶；
d)取环氧氯丙烷、高氯酸和无水乙醇，搅拌5-8min，再加入二氧化硅凝胶，25-28℃下静置10-12h，无水乙醇洗涤，再加入乙二胺无水乙醇混合溶液，置于50-55℃水浴下保温处理12-14h，再加入预处理阻燃内层，在35-40℃下浸泡2-3h，得到阻燃内层；
3)取待处理基布，置于聚氨酯树脂中浸泡5-10min，浸轧、焙烘，冷却至室温，得到基布；
4)取基布、阻燃内层、防火外层和粘结层，以自下而上为基布、粘结层、阻燃内层、粘结层、防火外层的排列顺序进行叠加，热压成型，成型温度为120-125℃，成型时间为12-14h，得到弹性面料。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115895193A (zh) * 2022-12-02 2023-04-04 山东莱蔚特复合材料有限责任公司 一种复合板簧用玻璃纤维增强树脂组合物的制备方法

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