CN117465088A - 一种消防服用防火阻燃多层复合面料及其制备方法 - Google Patents
一种消防服用防火阻燃多层复合面料及其制备方法 Download PDFInfo
- Publication number
- CN117465088A CN117465088A CN202311820110.8A CN202311820110A CN117465088A CN 117465088 A CN117465088 A CN 117465088A CN 202311820110 A CN202311820110 A CN 202311820110A CN 117465088 A CN117465088 A CN 117465088A
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- Prior art keywords
- fireproof
- flame
- heat
- fire
- layer
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- Granted
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Classifications
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Abstract
本发明属于消防复合面料技术领域，具体涉及一种消防服用防火阻燃多层复合面料及其制备方法。防火阻燃多层复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；防火耐磨层由聚丙烯腈预氧化纤维、改性玄武岩纤维混纺制得；防火保温隔热透气层由聚丙烯腈预氧化纤维、陶瓷纤维及隔热涂层组成；隔热涂层包括改性二氧化硅气凝胶和聚氨酯乳液；降温层由20‑30份水凝胶和70‑80份亲水性纤维复合得到；舒适层由芳纶非织造布组成；所制得的防火阻燃多层复合面料具有优异的阻燃、耐温、隔热、防护性能，能够进入大火中短时间工作，适用于消防用防护服。
Description
技术领域
本发明属于消防复合面料技术领域，具体涉及一种消防服用防火阻燃多层复合面料及其制备方法。
背景技术
阻燃防护服可以有效地防止火焰、高温和火花等危险物质对人体造成的伤害，通常用于消防员、冶金工人、炼油工人、电力工人、航天员等职业中,以确保他们在高温、高热或易燃环境下的安全，尤其对于消防服而言，其不仅要满足阻燃、稳定、绝热以及防止液体渗透等高标准要求，而且还要考虑热阻性能、抗划伤性能以及透气性、舒适度等因素，防止消防服在保护消防员的同时，给消防员带来不必要的负担和伤害。
申请号为201811508767.X的专利公开了一种消防服用阻燃面料及其制成的系列消防员穿着用品，阻燃面料采用以下原料按重量份混纺制成：芳纶纤维0-95，阻燃粘胶纤维25-50，腈氯纶纤维0-80，阻燃尼龙纤维0-20，导电纤维1-3，氨纶纤维0-10；通过多种阻燃纤维混纺得到的阻燃面料可以制成消防执勤服、消防作战训练服等消防员穿着用品，具有永久阻燃，不产生熔滴，抗静电性能好，强度高，耐磨性好，耐多种化学腐蚀，吸湿排汗性能好，抑菌防臭等诸多优点；申请号为202010214335.9的专利公开了一种消防服用高阻燃耐高温面料及其制备方法，其中高阻燃耐高温面料为三层面料，表层使用改性聚酰胺纤维的双股纱线作为表层的经、纬纱；中层的经纬纱线同样使用改性聚酰胺纤维的双股纱线；里层以羊绒纱线为经纱、大豆蛋白/棉混纺纱线作为纬纱；表层主要起阻燃作用，中层主要起隔热作用，里层贴近皮肤，为舒适层；所制得的面料具有较高的阻燃、耐温、隔热、防护性能，适用于消防用防护服。上述方案虽然都提供了阻燃作用的消防服面料，但阻燃效果具有一定的局限性，均不能达到进入火场短时间工作的防火效果。
发明内容
为了解决上述问题，本发明提供了一种消防服用防火阻燃多层复合面料及其制备方法，该防火阻燃多层复合面料包括防火耐磨层、防火保温隔热透气层、降温层、舒适层，具有优异的阻燃、耐温、隔热、防护性能，能够进入大火中短时间工作，适用于消防用防护服。
本发明为解决上述问题所采用的技术方案为：
一种消防服用防火阻燃多层复合面料的制备方法，所述复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；
所述防火耐磨层由聚丙烯腈预氧化纤维、改性玄武岩纤维混纺制得；
防火保温隔热透气层由聚丙烯腈预氧化纤维、陶瓷纤维及隔热涂层组成；所述隔热涂层包括改性二氧化硅气凝胶和聚氨酯乳液；
所述改性玄武岩纤维的制备方法为：将玄武岩纤维在丙酮中浸泡1-2h，再用水清洗干净，烘干后得到预处理的玄武岩纤维；将预处理的玄武岩纤维放入8-10%质量百分数的改性硅烷水溶液中，40-50℃下处理8-10h，取出烘干后得到改性玄武岩纤维；
所述改性硅烷的结构式为：
；
所述改性二氧化硅气凝胶的制备方法为：将正硅酸甲酯、改性硅烷加入到去离子水和无水乙醇的混合溶液中，搅拌混合均匀，然后加入0.5-1mol/L盐酸调节pH值为4-6，搅拌2-3h后，加入氨水调节pH值为8-10，缩合后得到湿凝胶，经超临界干燥得到改性二氧化硅气凝胶。
进一步地，所述改性硅烷的制备方法为：
S1、将对氨基苯甲酸、氯丙醇、三乙胺加入到乙醇中，升温至60-70℃，反应4-6h，得到化合物1，结构式为：
；所述对氨基苯甲酸、氯丙醇、三乙胺的摩尔比为1:1.1-1.2:1.5-1.2；
S2、将化合物1、三乙胺加入到无水乙醚中，冰浴条件下，滴加二乙基亚磷酰氯，滴毕，继续反应1-2h，得到化合物2，结构式为：
；所述化合物1、二乙基亚磷酰氯、三乙胺的摩尔比为1:1.1-1.2:1.5-2.0；
S3、将化合物2、三光气加入到四氢呋喃中，冰浴条件下，滴加吡啶，滴毕，室温反应8-10h，得到化合物3，结构式为：
；所述化合物2、三光气、吡啶的摩尔比为1:1.1-1.2:1.5-2.0；
S4、将3-氨基丙基三乙氧基硅烷加入到无水二氯甲烷中，氮气保护下，滴加含化合物3的二氯甲烷溶液，滴毕，30-35℃下反应2-4h，得到改性硅烷；所述3-氨基丙基乙甲氧基硅烷、化合物3的摩尔比为1:1-1.1。
进一步地，所述防火耐磨层由60-70份聚丙烯腈预氧化纤维、40-50份改性玄武岩纤维混纺制得；所述防火耐磨层的克重为200-250g/m2，厚度为0.5-0.7mm。
进一步地，所述防火保温隔热透气层的克重为300-350g/m2；先由50-60份聚丙烯腈预氧化纤维、30-40份陶瓷纤维混纺成厚度为1-2mm的纤维布，再将隔热涂层涂覆至纤维布上，烘干即得；隔热涂层的涂布厚度为0.4-0.5mm。
进一步地，所述隔热涂层的制备方法为：将聚氨酯乳液、助剂、粉碎后的改性二氧化硅气凝胶依次加入到去离子水中，分散均匀，得到隔热涂层；所述改性二氧化硅气凝胶、聚氨酯乳液、助剂、去离子水的质量比为1:15-20:0.1-0.2:20-25；所述助剂为聚羧酸钠盐。
进一步地，所述降温层由20-30份水凝胶和70-80份亲水性纤维复合得到；所述水凝胶为聚丙烯酸水凝胶、聚甲基丙烯脂水凝胶或聚丙烯酸胺水凝胶；所述亲水性纤维为阻燃维纶纤维、阻燃粘胶纤维或阻燃棉维；所述舒适层由芳纶非织造布组成。
本发明还提供了一种消防服用防火阻燃多层复合面料，经由上述所述的一种消防服用防火阻燃多层复合面料的制备方法制得。
本发明具有如下有益效果：
本发明以3-氨基丙基三乙氧基硅烷为原料，与含苯甲酰氯、亚磷酸酯基团的化合物3反应，得到了含亚磷酸酯基团的改性硅烷，所制得的改性硅烷具有双重阻燃作用，本发明将阻燃改性硅烷用于玄武岩纤维的表面改性，得到了改性玄武岩纤维，克服了玄武岩纤维由于表面呈惰性且光滑，难于与其他材料完美结合、发挥自身优异性能的缺陷，所制得的改性玄武岩纤维与聚丙烯腈预氧化纤维的相容性、结合力更好，两者混纺得到的防火耐磨层具有优异的阻燃隔热性能，断裂强力高，耐磨性较好；本发明还将阻燃改性硅烷、正硅酸甲酯水解缩聚，阻燃改性硅烷分子结构中的苯环长侧链，在缩聚过程中的支撑作用，有助于形成网状多空隙的改性二氧化硅气凝胶，所制备的改性二氧化硅气凝胶具有良好的保温隔热阻燃作用，进一步将其用作隔热涂层，成功制得了隔热、阻燃性能良好的防火保温隔热透气层。
本发明提供的防火阻燃多层复合面料包括防火耐磨层、防火保温隔热透气层、降温层、舒适层，具有优异的阻燃、耐温、隔热、防护性能，能够进入大火中短时间工作，适用于消防用防护服。
具体实施方式
下面将结合本申请实施例，对本申请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申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，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，都属于本申请保护的范围。
下述实施例中所用原料均为普通市售产品。其中，对氨基苯甲酸CAS号150-13-0；3-氯丙醇CAS号627-30-5；三乙胺CAS号121-44-8；二乙基亚磷酰氯CAS号589-57-1；三光气CAS号32315-10-9；吡啶CAS号110-86-1；3-氨基丙基三乙氧基硅烷CAS号919-30-2；乙醇CAS号64-17-5；二氯甲烷CAS号75-09-2；四氢呋喃CAS号109-99-9；乙醚CAS号60-29-7。
实施例1
本实施例提供一种消防服用防火阻燃多层复合面料的制备方法，复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；
其中防火耐磨层由70份聚丙烯腈预氧化纤维、50份改性玄武岩纤维混纺制得；防火耐磨层的克重为250g/m2，厚度为0.7mm。
防火保温隔热透气层由聚丙烯腈预氧化纤维、陶瓷纤维及隔热涂层组成；防火保温隔热透气层的克重为350g/m2；先由60份聚丙烯腈预氧化纤维、40份陶瓷纤维混纺成厚度为2mm的纤维布，再将隔热涂层涂覆至纤维布上，烘干即得；隔热涂层的涂布厚度为0.5mm。
降温层由30份水凝胶和80份亲水性纤维复合得到；水凝胶为聚丙烯酸水凝胶；亲水性纤维为阻燃维纶纤维；舒适层由芳纶非织造布组成，芳纶非织造布为芳纶1313。
改性玄武岩纤维的制备方法为：将玄武岩纤维在丙酮中浸泡2h，再用水清洗干净，烘干后得到预处理的玄武岩纤维；将预处理的玄武岩纤维放入10%质量百分数的改性硅烷水溶液中，50℃下处理8h，取出烘干后得到改性玄武岩纤维；
隔热涂层包括改性二氧化硅气凝胶和聚氨酯乳液；制备方法为：将聚氨酯乳液、助剂、粉碎后的改性二氧化硅气凝胶依次加入到去离子水中，分散均匀，得到隔热涂层；改性二氧化硅气凝胶、聚氨酯乳液、助剂、去离子水的质量比为1:20:0.2:25；助剂为聚羧酸钠盐。
改性二氧化硅气凝胶的制备方法为：将正硅酸甲酯、改性硅烷加入到去离子水和无水乙醇的混合溶液中，搅拌混合均匀，然后加入1mol/L盐酸调节pH值为6，搅拌3h后，加入氨水调节pH值为10，缩合后得到湿凝胶，经超临界干燥得到改性二氧化硅气凝胶。
改性硅烷的制备方法为：
S1、将27.5g对氨基苯甲酸、20.9g氯丙醇、30.4g三乙胺加入到800mL乙醇中，升温至70℃，反应6h，反应完成后，自然降至室温，除去乙醇，用800mL水和800mL二氯甲烷进行萃取，收集有机相，干燥后减压浓缩得到32.6g化合物1；对氨基苯甲酸、氯丙醇、三乙胺的摩尔比为1:1.1:1.5；反应过程为：
；
化合物1：ESI(m/z)：196.1[M+H]+，1H-NMR(600MHz，DMSO-d6，δppm)：12.71（s，1H），7.84（d，J=8.6Hz，2H），6.88（d，J=8.6Hz，2H），6.43（s，1H），4.74（s，1H），3.46-3.49（m，4H），1.76-1.78（m，2H）。
S2、将25.0g化合物1、19.4g三乙胺加入到650mL无水乙醚中，冰浴条件下，滴加22.1g二乙基亚磷酰氯，滴毕，继续反应2h，反应完成后，除去乙醚，加入600mL水和600mL二氯甲烷进行萃取，收集有机相，干燥后减压浓缩得到33.5g化合物2，化合物1、二乙基亚磷酰氯、三乙胺的摩尔比为1:1.1:1.5；反应过程为：
；
化合物2：ESI(m/z)：316.1[M+H]+，1H-NMR(600MHz，DMSO-d6，δppm)：12.72（s，1H），7.85（d，J=8.6Hz，2H），6.86（d，J=8.6Hz，2H），6.42（s，1H），3.80-3.84（m，6H），3.41-3.43（m，2H），1.76-1.78（m，2H），1.25（t，J=7.2Hz，6H）。
S3、将25.0g化合物2、25.9g三光气加入到400mL四氢呋喃中，冰浴条件下，滴加12.6g吡啶，滴毕，室温反应10h，反应完成后，抽滤，滤液减压浓缩得到22.8g化合物3，化合物2、三光气、吡啶的摩尔比为1:1.1:2.0；反应过程为：
；
化合物3：ESI(m/z)：334.1[M+H]+，1H-NMR(600MHz，DMSO-d6，δppm)：8.01（d，J=8.6Hz，2H），6.88（d，J=8.6Hz，2H），6.43（s，1H），3.80-3.84（m，6H），3.41-3.43（m，2H），1.76-1.78（m，2H），1.25（t，J=7.2Hz，6H）。
S4、将13.3g 3-氨基丙基三乙氧基硅烷加入到200mL无水二氯甲烷中，氮气保护下，滴加含20.0g化合物3的100mL二氯甲烷溶液，滴毕，30-35℃下反应2-4h，反应完成后，自然降至室温，除去二氯甲烷，得到25.7g改性硅烷；3-氨基丙基乙甲氧基硅烷、化合物3的摩尔比为1:1；反应过程为：
；
改性硅烷：ESI(m/z)：519.2[M+H]+，1H-NMR(600MHz，DMSO-d6，δppm)：8.44（s，1H），7.59（d，J=8.6Hz，2H），6.85（d，J=8.6Hz，2H），6.43（s，1H），3.83-3.85（m，12H），3.41-3.43（m，4H），1.65-1.71（m，4H），1.21-1.25（m，15H），0.56-0.60（m，2H）。
实施例2
本实施例提供一种消防服用防火阻燃多层复合面料的制备方法，复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；
其中防火耐磨层由60份聚丙烯腈预氧化纤维、40份改性玄武岩纤维混纺制得；防火耐磨层的克重为200g/m2，厚度为0.5mm。
防火保温隔热透气层由聚丙烯腈预氧化纤维、陶瓷纤维及隔热涂层组成；防火保温隔热透气层的克重为300g/m2；先由50份聚丙烯腈预氧化纤维、30份陶瓷纤维混纺成厚度为1mm的纤维布，再将隔热涂层涂覆至纤维布上，烘干即得；隔热涂层的涂布厚度为0.4mm。
降温层由20份水凝胶和70份亲水性纤维复合得到；水凝胶为聚甲基丙烯脂水凝胶；亲水性纤维为阻燃粘胶纤维；舒适层由芳纶非织造布组成，芳纶非织造布为芳纶1313。
改性玄武岩纤维的制备方法为：将玄武岩纤维在丙酮中浸泡1h，再用水清洗干净，烘干后得到预处理的玄武岩纤维；将预处理的玄武岩纤维放入8%质量百分数的改性硅烷水溶液中，40℃下处理10h，取出烘干后得到改性玄武岩纤维；
隔热涂层包括改性二氧化硅气凝胶和聚氨酯乳液；制备方法为与实施例1相同。
改性二氧化硅气凝胶的制备方法为与实施例1相同。
实施例3
本实施例提供一种消防服用防火阻燃多层复合面料的制备方法，复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；
其中防火耐磨层由60份聚丙烯腈预氧化纤维、50份改性玄武岩纤维混纺制得；防火耐磨层的克重为200g/m2，厚度为0.7mm。
防火保温隔热透气层由聚丙烯腈预氧化纤维、陶瓷纤维及隔热涂层组成；防火保温隔热透气层的克重为300g/m2；先由50份聚丙烯腈预氧化纤维、40份陶瓷纤维混纺成厚度为1.5mm的纤维布，再将隔热涂层涂覆至纤维布上，烘干即得；隔热涂层的涂布厚度为0.5mm。
降温层由25份水凝胶和75份亲水性纤维复合得到；水凝胶为聚丙烯酸胺水凝胶；亲水性纤维为阻燃棉维；舒适层由芳纶非织造布组成，芳纶非织造布为芳纶1313。
改性玄武岩纤维的制备方法与实施例1相同。
隔热涂层包括改性二氧化硅气凝胶和聚氨酯乳液；制备方法为：将聚氨酯乳液、助剂、粉碎后的改性二氧化硅气凝胶依次加入到去离子水中，分散均匀，得到隔热涂层；改性二氧化硅气凝胶、聚氨酯乳液、助剂、去离子水的质量比为1:15:0.1:20；助剂为聚羧酸钠盐。
改性二氧化硅气凝胶的制备方法为与实施例1相同。
对比例1
本对比例提供一种消防服用防火阻燃多层复合面料的制备方法，复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；
其中防火耐磨层由70份聚丙烯腈预氧化纤维、50份玄武岩纤维混纺制得；防火耐磨层的克重为250g/m2，厚度为0.7mm。
防火保温隔热透气层、降温层、舒适层与实施例1相同。
隔热涂层及其制备方法、改性二氧化硅气凝胶的制备方法均与实施例1相同。
对比例2
本实施例提供一种消防服用防火阻燃多层复合面料的制备方法，复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；
其中防火耐磨层与实施例1相同。
防火保温隔热透气层由聚丙烯腈预氧化纤维、陶瓷纤维及隔热涂层组成；防火保温隔热透气层的克重为350g/m2；先由60份聚丙烯腈预氧化纤维、40份陶瓷纤维混纺成厚度为2mm的纤维布，再将隔热涂层涂覆至纤维布上，烘干即得；隔热涂层的涂布厚度为0.5mm。
降温层、舒适层与实施例1相同。
改性玄武岩纤维的制备方法与实施例1相同。
隔热涂层包括二氧化硅气凝胶和聚氨酯乳液；制备方法为：将聚氨酯乳液、助剂、粉碎后的二氧化硅气凝胶依次加入到去离子水中，分散均匀，得到隔热涂层；二氧化硅气凝胶、聚氨酯乳液、助剂、去离子水的质量比为1:20:0.2:25；助剂为聚羧酸钠盐。
二氧化硅气凝胶的制备方法为：将正硅酸甲酯、3-氨基丙基三乙氧基硅烷加入到去离子水和无水乙醇的混合溶液中，搅拌混合均匀，然后加入1mol/L盐酸调节pH值为6，搅拌3h后，加入氨水调节pH值为10，缩合后得到湿凝胶，经超临界干燥得到二氧化硅气凝胶。
性能测试
对实施例1-3及对比例1-2所制得的防火耐磨层、防火保温隔热透气层及防火阻燃多层复合面料进行性能测试，其中，极限氧指数参照GB/T5454-1997标准；经向拉伸断裂强力参照GB/T3923.1-2013标准；隔热效果参照GB/T22588-2008标准；燃烧性能参照GB/T5455-2014标准，试样尺寸300×80mm，火焰高度4cm，试样点燃时间12s，记录续燃时间和阴燃时间；卸下试样后，沿长度方向将炭化处对折，在下端距其底边及侧边各6mm处，挂上重锤，提起试样下端的另一侧至重锤悬空，得到试样撕裂的长度，即为损毁长度；防火耐磨层的测试结果如表1所示，防火保温隔热透气层的测试结果如表2所示，防火阻燃多层复合面料的测试结果如表3所示。
表1防火耐磨层的测试结果
由表1结果可知，由实施例1-3制得的防火耐磨层具有较高的极限氧指数、断裂强力，25℃、300℃的导热系数较低，说明防火耐磨层的保温隔热性好，与对比例1相比，实施例1中使用改性玄武岩纤维与聚丙烯腈预氧化纤维混纺，玄武岩纤维表面经过阻燃改性硅烷改性后，与聚丙烯腈预氧化纤维之间的结合力更好，从而得到了综合性能较好的防火耐磨层。
表2防火保温隔热透气层的测试结果
由表2结果可知，由实施例1-3制得的防火保温隔热透气层具有较高的极限氧指数、25℃、300℃的导热系数较低，说明防火保温隔热透气层的保温隔热性好，与对比例2相比，实施例1中使用的隔热涂层由改性二氧化硅气凝胶和聚氨酯乳液制得，改性二氧化硅气凝胶以正硅酸甲酯、阻燃改性硅烷为原料制得，本发明所制得的改性二氧化硅气凝胶的隔热、阻燃性能更好，将其用于隔热涂层，从而提高了防火保温隔热透气层的隔热、阻燃性能。
表3防火阻燃多层复合面料的测试结果
由表3结果可知，由实施例1-3制得的防火阻燃多层复合面料的续燃时间、阴燃时间及损毁长度均为0，无滴落熔融现象，说明该防火阻燃多层复合面料具有优异的阻燃性能；与对比例1-2相比，实施例1中由改性玄武岩纤维与聚丙烯腈预氧化纤维混纺而成的防火耐磨层，表层涂覆含改性二氧化硅气凝胶隔热涂层的防火保温隔热透气层，两者复合作为消防服的外层能够起到很好地阻燃隔热作用。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本申请的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本申请的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本申请的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，所述复合面料由外向内依次由防火耐磨层、防火保温隔热透气层、降温层、舒适层绗缝合制得；
所述防火耐磨层由聚丙烯腈预氧化纤维、改性玄武岩纤维混纺制得；
防火保温隔热透气层由聚丙烯腈预氧化纤维、陶瓷纤维及隔热涂层组成；所述隔热涂层包括改性二氧化硅气凝胶和聚氨酯乳液；
所述改性玄武岩纤维的制备方法为：将玄武岩纤维在丙酮中浸泡1-2h，再用水清洗干净，烘干后得到预处理的玄武岩纤维；将预处理的玄武岩纤维放入8-10%质量百分数的改性硅烷水溶液中，40-50℃下处理8-10h，取出烘干后得到改性玄武岩纤维；
所述改性硅烷的结构式为：
；
所述改性二氧化硅气凝胶的制备方法为：将正硅酸甲酯、改性硅烷加入到去离子水和无水乙醇的混合溶液中，搅拌混合均匀，然后加入0.5-1mol/L盐酸调节pH值为4-6，搅拌2-3h后，加入氨水调节pH值为8-10，缩合后得到湿凝胶，经超临界干燥得到改性二氧化硅气凝胶。
2.根据权利要求1所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，所述改性硅烷的制备方法为：
S1、将对氨基苯甲酸、氯丙醇、三乙胺加入到乙醇中，升温至60-70℃，反应4-6h，得到化合物1，结构式为：
；
S2、将化合物1、三乙胺加入到无水乙醚中，冰浴条件下，滴加二乙基亚磷酰氯，滴毕，继续反应1-2h，得到化合物2，结构式为：
；
S3、将化合物2、三光气加入到四氢呋喃中，冰浴条件下，滴加吡啶，滴毕，室温反应8-10h，得到化合物3，结构式为：
；
S4、将3-氨基丙基三乙氧基硅烷加入到无水二氯甲烷中，氮气保护下，滴加含化合物3的二氯甲烷溶液，滴毕，30-35℃下反应2-4h，得到改性硅烷。
3.根据权利要求2所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，步骤S1中所述对氨基苯甲酸、氯丙醇、三乙胺的摩尔比为1:1.1-1.2:1.5-1.2；步骤S2中所述化合物1、二乙基亚磷酰氯、三乙胺的摩尔比为1:1.1-1.2:1.5-2.0。
4.根据权利要求2所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，步骤S3中所述化合物2、三光气、吡啶的摩尔比为1:1.1-1.2:1.5-2.0；步骤S4中所述3-氨基丙基乙甲氧基硅烷、化合物3的摩尔比为1:1-1.1。
5.根据权利要求1所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，所述防火耐磨层由60-70份聚丙烯腈预氧化纤维、40-50份改性玄武岩纤维混纺制得；所述防火耐磨层的克重为200-250g/m2，厚度为0.5-0.7mm。
6.根据权利要求1所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，所述防火保温隔热透气层的克重为300-350g/m2；先由50-60份聚丙烯腈预氧化纤维、30-40份陶瓷纤维混纺成厚度为1-2mm的纤维布，再将隔热涂层涂覆至纤维布上，烘干即得；隔热涂层的涂布厚度为0.4-0.5mm。
7.根据权利要求6所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，所述隔热涂层的制备方法为：将聚氨酯乳液、助剂、粉碎后的改性二氧化硅气凝胶依次加入到去离子水中，分散均匀，得到隔热涂层。
8.根据权利要求7所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，所述改性二氧化硅气凝胶、聚氨酯乳液、助剂、去离子水的质量比为1:15-20:0.1-0.2:20-25；所述助剂为聚羧酸钠盐。
9.根据权利要求1所述的一种消防服用防火阻燃多层复合面料的制备方法，其特征在于，所述降温层由20-30份水凝胶和70-80份亲水性纤维复合得到；所述水凝胶为聚丙烯酸水凝胶、聚甲基丙烯脂水凝胶或聚丙烯酸胺水凝胶；所述亲水性纤维为阻燃维纶纤维、阻燃粘胶纤维或阻燃棉维；所述舒适层由芳纶非织造布组成。
10.一种消防服用防火阻燃多层复合面料，其特征在于，经由权利要求1-9任一项所述的一种消防服用防火阻燃多层复合面料的制备方法制得。
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| CN117944337A (zh) * | 2024-03-27 | 2024-04-30 | 成都鲲鹏云智科技有限公司 | 一种阻燃隔热复合纤维面料及其制备方法、在防火服中的应用 |
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