棉织物耐久阻燃剂的制备与应用
摘要
本文主要研究了棉用耐久阻燃剂N-羟甲基-3-二甲基膦丙酰胺的合成工艺及其在棉织物上的阻燃应用工艺，找出了合成的最佳工艺路线和阻燃应用较为成熟的工艺条件，具体内容如下：
1．用无溶剂法合成了棉用耐久阻燃剂，并采用一种新的催化体系对反应进行催化，通过对反应物的物料比、反应时间、反应pH值、反应温度等条件的考察，找出了其最佳合成工艺，不但使产物的转化率提高到98.1％，比文献报道的78％增加了20％，而且使传统催化剂甲醇钠的用量降为文献报道的1／3；阻燃剂中游离甲醛的含量从1.13％降到0.42％。
2．用合成的阻燃剂对棉织物进行阻燃整理。通过正交试验找出了阻燃整理工艺中的各种基本因素(阻燃剂、交联剂、催化剂)对织物阻燃性能的影响，确定了最佳阻燃整理工艺；按照AATCC水洗要求对织物洗涤50次以上，织物仍然具有较好的阻燃性能，说明该阻燃剂还具有较好的耐洗性。
3．通过改进工艺条件、改变整理工艺以及添加剂的使用，整理后的织物色变小，手感好，并且有效地改降低了阻燃整理后织物上的游离甲醛含量，仅为30mg／kg，大大低于文献报道的300mg／kg；织物的断裂强力损失也降至20％，比文献值降低了近15％，具有更大的应用价值。
The flame retardant finishing of pure cotton fibric N-hydroxymethyl-3-dimethoxyl phosphinylidyne propionylamide was synthesized; at the same time, the optimal synthesis conditions had been selected from the design. The optimal flame retardant finishing technology was obtained in the application of flame retardant to pure cotton fabric. The main points were as follows:
1. A new catalyst system was applied in this reaction. The reaction conditions were investigated in the synthesis reaction. In this condition,the conversion of the product was improved to 98.1%,which was much more than 78% reported in the literature; The dosage of catalyst sodium methylate (in methanol) was reduced to the 1/3 of the dosage before; The content of the dissociated formaldehyde was reduced from 1.13% to 0.42% .
2. The optimal process conditions of flame retardant finishing of pure cotton were determined through orthogonal experiment .The dosage of the flame retardant, cross linking agent and catalyst was investigated. The results showed that the cotton fabric of flame retardant finishing had durable flame retardancy property and washability without adverse effects on the original style of the finished fabric and its inherent quality. The cotton fabric still had superior flame retardancy after washing more than 50 times.
3. After improving the conditions of the finishing technology and using the additives, the content of the dissociated formaldehyde in the finished pure cotton fabric fell to 30mm/kg effectively, which was much lower than 300mm/kg reported in the literature; The loss of the strength of the cotton fabric reached about 20%, as well as good flame resistance, soft handle, and excellent washability.
1．用无溶剂法合成了棉用耐久阻燃剂，并采用一种新的催化体系对反应进行催化，通过对反应物的物料比、反应时间、反应pH值、反应温度等条件的考察，找出了其最佳合成工艺，不但使产物的转化率提高到98.1％，比文献报道的78％增加了20％，而且使传统催化剂甲醇钠的用量降为文献报道的1／3；阻燃剂中游离甲醛的含量从1.13％降到0.42％。
2．用合成的阻燃剂对棉织物进行阻燃整理。通过正交试验找出了阻燃整理工艺中的各种基本因素(阻燃剂、交联剂、催化剂)对织物阻燃性能的影响，确定了最佳阻燃整理工艺；按照AATCC水洗要求对织物洗涤50次以上，织物仍然具有较好的阻燃性能，说明该阻燃剂还具有较好的耐洗性。
3．通过改进工艺条件、改变整理工艺以及添加剂的使用，整理后的织物色变小，手感好，并且有效地改降低了阻燃整理后织物上的游离甲醛含量，仅为30mg／kg，大大低于文献报道的300mg／kg；织物的断裂强力损失也降至20％，比文献值降低了近15％，具有更大的应用价值。
The flame retardant finishing of pure cotton fibric N-hydroxymethyl-3-dimethoxyl phosphinylidyne propionylamide was synthesized; at the same time, the optimal synthesis conditions had been selected from the design. The optimal flame retardant finishing technology was obtained in the application of flame retardant to pure cotton fabric. The main points were as follows:
1. A new catalyst system was applied in this reaction. The reaction conditions were investigated in the synthesis reaction. In this condition,the conversion of the product was improved to 98.1%,which was much more than 78% reported in the literature; The dosage of catalyst sodium methylate (in methanol) was reduced to the 1/3 of the dosage before; The content of the dissociated formaldehyde was reduced from 1.13% to 0.42% .
2. The optimal process conditions of flame retardant finishing of pure cotton were determined through orthogonal experiment .The dosage of the flame retardant, cross linking agent and catalyst was investigated. The results showed that the cotton fabric of flame retardant finishing had durable flame retardancy property and washability without adverse effects on the original style of the finished fabric and its inherent quality. The cotton fabric still had superior flame retardancy after washing more than 50 times.
3. After improving the conditions of the finishing technology and using the additives, the content of the dissociated formaldehyde in the finished pure cotton fabric fell to 30mm/kg effectively, which was much lower than 300mm/kg reported in the literature; The loss of the strength of the cotton fabric reached about 20%, as well as good flame resistance, soft handle, and excellent washability.
引文
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