【作者】 孙兵；

【导师】 周向东；

【作者基本信息】 苏州大学 ， 纺织化学与染整工程， 2015， 硕士

【摘要】 锦纶是世界上最早实现工业化生产的合成纤维,在合成纤维中产量居第二位,与其他合成纤维相比,锦纶纤维具有耐磨性好、回弹性高、断裂强度高、染色性好、比重小以及不易虫蛀等优点。但锦纶的热性能并不好,其易燃烧性能以及燃烧过程中产生的熔融滴落物易造成火势蔓延等缺点,限制了它的广泛应用。但是到目前为止,市场上用于锦纶后整理的阻燃产品寥寥无几。针对上述这些问题,本课题合成了两种阻燃剂,一种是交联型含硫磷酰胺类阻燃剂,另一种是共晶型含酰胺链段阻燃剂。并且将它们应用于锦纶织物整理上,具体研究内容如下:以多聚磷酸(PPA)、环氧氯丙烷(EC)为原料,在催化剂无水三氯化铝(AT)的作用下合成中间体磷酸单酯(PHME);以二环己基碳二亚胺(DCC)为缩合剂,PHME与硫脲(TU)反应得到最终目标产物含硫磷酰胺阻燃剂(FRS)。利用红外光谱(FRIR)、核磁共振(1HNMR)和热重分析(TG-DTA)表征了产物的结构与性能,并优化了合成工艺,中间体磷酸单酯(PHME)的合成:n(PPA):n(EC)=1.5:1,催化剂用量为2%,反应温度80℃,反应时间为3h;目标产物阻燃剂(FRS)的合成:n(PHME):n(TU)=1:1.1,缩合剂二环己基碳二亚胺(DCC)用量为1.5%,反应温度110℃,反应时间为2h。以自制的封端异氰酸酯做交联剂,将合成的阻燃剂应用于锦纶织物的阻燃整理,当阻燃剂用量为200g/L,交联剂用量为40g/L,焙烘温度为150℃,焙烘时间为3h,整理后锦纶织物的极限氧指数为34.1%,损毁炭长为5.7cm,水洗10次之后,极限氧指数为28.5%,损毁炭长为7.7cm。结合烟密度分析、MCC分析与XPS织物表面元素分析测试,合成的交联型含硫磷酰胺阻燃剂对锦纶织物具有较好的耐久阻燃效果。以己二酸(AA)、己二胺(HAD)为原料,以无水乙醇为溶剂,合成初始单体PA66盐;以五氧化二磷、硫脲(TU)为原料,合成阻燃单体(FR);在缩合剂DCC的催化作用下,FR与PA66缩合得到最终目标产物含酰胺共晶链段阻燃剂(PA-FR)。利用红外光谱(FRIR)、核磁共振(1HNMR)和热重分析(TG-DTA)表征了产物的结构与性能,并优化了合成工艺:m(FR):m(PA66)=2.5:1,缩合剂DCC用量为2%,反应温度为110℃,反应时间为3.5h。将合成的阻燃剂应用于锦纶织物的阻燃整理,当阻燃剂用量为200g/L,p H值为7,焙烘温度为150℃,焙烘时间为3min,整理后锦纶织物的极限氧指数为30.4%,损毁炭长为7.1cm,水洗10次之后,极限氧指数为26.8%,损毁炭长为9.4cm。结合SEM图与X-射线衍射分析测试表明,共晶型含酰胺链段阻燃剂与锦纶织物产生了较好的共晶作用,对锦纶织物具有一定的耐久阻燃效果。更多还原

【Abstract】 Nylon is one of the most used polymers for synthetic fibers, and nylon production ranks the second place in the synthetic fiber. Comparison with other fibers, nylon fiber has many advantages, such as good abrasion resistance, high elastic resilience, high breaking strength,excellent dyeing properties, the specific gravity small and no worm, etc. But thermal performance of nylon is poor, the ignitability and molten droplets in the combustion process of nylon easily make fire to spread, which is very unfavorable for fire-fighting. In a word, the drawbacks of nylon seriously limited the extensive application. But so far,flame-retardants used in finishing are few on the market. Aiming at these problems, two kinds of flame-retardants are studies, one was a crosslinked sulfur-containing phosphoric amide flame-retardant. Another was an eutectic amide-containing flame-retardant. And they were used in flame retardant finishing on nylon fabric, contents and results of study are as follows:Using the anhydrous aluminum chloride as the catalyst, the phosphate monoester(PHME)was synthesized by polyphosphoric acid(PPA) and epoxy chloropropane(EC). Using DCC as the condensing agent, the sulfur-containing phosphoric amide flame-retardant(FRS) was synthesized by PHME and thiourea(TU). The structures and properties were studied by FTIR,1HNMR and TG-DTA. The optimal synthetic conditions of PHME were as follows:n(PPA) : n(EC) = 1.5:1, catalyst was was 2%, the temperature was 80℃ and the reaction time was 3h. The optimal synthetic conditions of FRS were as follows: n(PHME) : n(TU)= 1:1.1, catalyst was was 1.5%, the temperature was 110℃and the reaction time was 2h.With the water-soluble isocyanate-terminated as cross-linker, the flame retardant was applied to flame retardant finishing on nylon fabric. Finally, the test indicated that the LOI value and damaged carbon length of the finished nylon fabric were 34.1% and 5.7 cm,respectively, when the concentration value of FRS and WIT were 200 g/L and 40 g/L,respectively, and the baking temperature and time were 150℃ and 3 min, respectively.After 10 laundry cycles, the LOI value and damaged carbon length of the finished nylon fabric were 28.5% and 7.7 cm. The test indicated that the FRS has good durable flame retardancy.Using the ethanol as the solvent, the PA66 was synthesized by adipic acid(AA) and hexamethylene diamine(HAD). Using DCC as the condensing agent, the FR was synthesized by pentoxide and thiourea(TU). The eutectic amide-containing flame-retardant(PA-FR) was synthesized by PA66 and FR. The structures and properties were studied by FTIR,1HNMR and TG-DTA. The optimal synthetic conditions of PA-FR were as follows: m(FR) : m(PA66) = 2.5 : 1, catalyst was was 2%, the temperature was110℃ and the reaction time was 3.5h. Finally, the test indicated that the LOI value and damaged carbon length of the finished nylon fabric were 30.4% and 7.1 cm, respectively,when the concentration value and p H of PA-FR were 200 g/L and 7, respectively, and the baking temperature and time were 150℃ and 3 min, respectively. After 10 laundry cycles,the LOI value and damaged carbon length of the finished nylon fabric were 26.8% and 9.4cm. The test indicated that the PA-FR has some durable flame retardancy.更多还原