磷腈系抗菌阻燃蛋白粘胶纤维的研究
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摘要
随着科学技术的发展和消费水平的提高，人们对阻燃粘胶纤维及其制品的需求量和其使用性能的要求都不断提高。因此，阻燃粘胶纤维的发展不仅要求使用环境友好型阻燃剂，而且要具有良好的服用性及抗菌、抑菌性。然而，目前将这几种功能结合在一起的多功能复合型粘胶纤维的研究还未见报道。本文以六苯氧基环三磷腈（hexaphenoxycyclotriphosphazene，HPTP）这种符合环保要求的磷腈衍生物为阻燃剂制备了阻燃粘胶纤维。在湿法纺丝过程中添加动物蛋白胶液，制备了阻燃蛋白粘胶纤维。应用壳聚糖抗菌剂对纤维进行整理，在国内首次制备了抗菌阻燃蛋白粘胶纤维。系统地研究了这几种粘胶纤维的阻燃性能、机械强度和服用性等性能。
本文将HPTP应用于粘胶纤维的阻燃研究。以六氯环三磷腈和苯酚钠为反应物，制备了HPTP。采用正交试验法研究了反应过程中温度、反应时间和投料比对产物产率的影响，得到了制备苯氧基磷腈的最佳合成工艺，产率为76.52%，加入聚乙二醇脂肪酸酯催化剂后，达到97.3%。所得产物的红外光谱图和31P核磁共振谱证明产物为取代完全的HPTP。差示扫描量热法（DSC）和热重分析（TG）的结果表明HPTP比HCTP的分解温度提高了约250℃，是耐热性更好的阻燃材料。
在将HPTP应用于湿法纺丝前，本文通过正交试验法选择了APG/EL-20乳化分散体系，解决了HPTP颗粒大、分散性不好的问题，使阻燃剂在湿法纺丝过程中与粘胶纺丝液混合均匀，在阻燃粘胶纤维断面上可看到形成了分布均匀的绒毛状结构。采用扫描电镜法、极限氧指数（LOI）法、45度燃烧法、差示扫描量热法（DSC）、热重分析（TG）法等方法测试了阻燃粘胶纤维的燃烧性能和热稳定性。随着阻燃剂含量的增加，其阻燃效果明显增强，含16%阻燃剂的阻燃粘胶纤维LOI值为28.5%，接火3次以上，燃烧失重率为21.12%，属于难燃纤维，经30次水洗测试仍保持阻燃效果。阻燃剂的加入使粘胶纤维的第一次分解温度提前约20℃，分解速度加快；二次碳化时变得困难，第二次分解速度变缓，碳化温度滞后约30~50℃。纤维燃烧后表面生成碳化层，保留了纤维的结构。
首先采用共混法将蛋白液、阻燃剂与粘胶纺丝液共混制备出阻燃蛋白粘胶纤维。在阻燃剂添加量保持在16%的基础上再加入5%的动物蛋白，通过SEM观察发现制得的阻燃蛋白粘胶纤维内部结构更加紧密，纤维表面出现了均匀散状分布的小孔；经LOI及45度燃烧测试，30次水洗前后的阻燃蛋白粘胶纤维均能达到难燃纤维标准。性能测试表明，阻燃蛋白粘胶纤维的主要改善是取向度、机械强度明显提高，回潮率比普通粘胶纤维略差，但较阻燃粘胶纤维的回潮率大13.3%，保温性有所提高；摩擦系数较阻燃粘胶纤维要小；膨松度提高，并超过普通粘胶纤维；在后加工过程中通过改性氨基有机硅柔软剂进行表面改性得到了具有丝滑手感的纤维。
采用表面抗菌整理的方法将壳聚糖及纳米银-壳聚糖复合抗菌整理液应用到阻燃蛋白粘胶纤维中。处理后的抗菌阻燃蛋白粘胶纤维对混合菌的抑菌率分别达92.4%和97.6%，水洗30次后仍能达到89.3%和93.8%。纤维水洗前后LOI值均保持在29%以上，通过氮元素含量的测定发现了阻燃效果叠加规律；抗菌整理后的纤维干强比抗菌整理前有所提高，比普通粘胶纤维低，湿强则较普通粘胶纤维高；摩擦系数较抗菌整理前增大；通过改性氨基有机硅柔软剂的柔软整理，使最终制备的纤维摩擦系数低于普通粘胶纤维的摩擦系数，使最终样品的阻燃性能、机械强度、服用性能、抗菌性能都达到最优。
The demands of quantity and quality of flame-retardant textiles increasedramatically with the rapid development of technology and the booming consumptionlevel. In viscose fiber industry, environemental-firendly flame retardants are required, aswell as excellent wearing performance and antibacterial property. However,multi-functional product with combined features has not been reported. In this paper,flame-retardant viscose fiber was prepared by the addition of an environment-friendlyphosphazene derivative, hexaphenoxycyclotriphosphazene (HPTP). Flame-retardantprotein viscose fiber was prepared by adding animal protein solution to spinning solution.By using chitosan as antibacterial agent, Antibacterial flame-retardant protein viscosefiber was prepared for the first time. Flame retardancy, mechanical strength, wearingperformance and other properties of these viscose fibers were studied systematically.
In this paper, HPTP was applied to the study of flame-retardant viscose fiber for thefirst time. Sodium phenate and hexachlorocyclotriphosphazene (HCTP) were used asreactants to synthesize HPTP. Reaction factors such as temperature, time and reactantratio were optimized using orthogonal test design, which gave a yield of76.52%. A yieldof97.3%was accomplished after PEG400was added as catalyst. Infrared spectrum and31P NMR spectrum were employed to characterize and determine the structure of theproduct. Results showed that Cl atoms were replaced completely. Differential scanningcalorimetry (DSC) and Thermogravimetry (TG) results indicated that the decompositiontemperature of HPTP is250degree centigrade higher than that of HCTP. It proved thatHPTP is a flame retardant with better heat-resistance.
APG/EL-20emulsification system was selected and optimized using orthogonal testdesign to solve the bad dissolubility of HPTP before wet spinning. HPTP was blendedwith viscose spinning solution thoroughly. Fluffy structures spread uniformly wereobserved on the cross section of flame-retardant viscose fiber. The igniting property andthermal stability of the samples were evaluated by scanning electron microscope (SEM),Limited oxygen index (LOI),45degree igniting test, DSC, TG. The results indicated thathigher flame retardant percentage fiber has better flame retardancy. Viscose fiber with 16%flame retardant was evaluated as flame-retardant fiber (LOI=28.5%, ignition time>3, ignition weight loss=21.12%). The flame retardancy of the fiber remained after30times wash test. The first decomposition temperature of flame-retardant viscose fiber wasdecreased by20degree centigrade, decomposition rate was accelerated. Secondarycarbonization was more difficult than beforedecomposition rate was slower and the peakof decomposition was lagged by30~50degree centigrade. After igniting test, carbonizedlayer was formed on the surface of flame-retardant viscose fiber, the structure of fiberremained. Mechanical strength of the fiber with our emulsification system performedbetter than viscose fiber with common emulsification system.
Protein solution, flame retardant and viscose spinning solution were blended for thefirst time to prepare flame-retardant protein viscose fiber. Animal protein was added5%by weight to spinning solution on the basis of16%flame retardant. The product has morecompact structure inside the fiber and evenly scattered small pores on the surface. Resultsof LOI and45degree igniting test showed that the flame-retardant protein viscose fibercan reach the flame-retardant standard both before and after30times wash test. The chiefimprovement of this product is the better orientation and mechanical strength. Moistureregain of the fiber is a little lower than that of normal viscose fiber, however, it is13.3%higher than the moisture regain of flame-retardant viscose fiber, heat retention is alsoimproved. Friction coefficient of the product is lower than that of flame-retardant viscosefiber. Bulking intensity is increased, better than that of normal viscose fiber. The productwas modified with modified amino organic silicon softener to obtain silk-like feel.
Chitosan and Ag nanoparticles-chitosan antibacterial agent were used to finish theflame-retardant protein viscose fiber. After modification the antibacterial flame-retardantprotein viscose fiber showed92.4%and97.6%inhibition to mixed strain,89.3%and93.8%after30times wash teat, respectively. LOI of the product is higher than29%before and after wash test. The improvement of the flame retardanc is based on theaccumulation of N element. Dry mechanical strength of the fiber is increased while stilllower than normal viscose fiber. However, the wet mechanical strength is much improvedthan that of normal viscose fiber. Friction coefficient is increased. After modification byusing modified amino organic silicon softener, the friction coefficient is lower than that of normal viscose fiber. The final product has optimized flame retardancy, mechanicalstrength, wearing performance and antibacterial function.
本文将HPTP应用于粘胶纤维的阻燃研究。以六氯环三磷腈和苯酚钠为反应物，制备了HPTP。采用正交试验法研究了反应过程中温度、反应时间和投料比对产物产率的影响，得到了制备苯氧基磷腈的最佳合成工艺，产率为76.52%，加入聚乙二醇脂肪酸酯催化剂后，达到97.3%。所得产物的红外光谱图和31P核磁共振谱证明产物为取代完全的HPTP。差示扫描量热法（DSC）和热重分析（TG）的结果表明HPTP比HCTP的分解温度提高了约250℃，是耐热性更好的阻燃材料。
在将HPTP应用于湿法纺丝前，本文通过正交试验法选择了APG/EL-20乳化分散体系，解决了HPTP颗粒大、分散性不好的问题，使阻燃剂在湿法纺丝过程中与粘胶纺丝液混合均匀，在阻燃粘胶纤维断面上可看到形成了分布均匀的绒毛状结构。采用扫描电镜法、极限氧指数（LOI）法、45度燃烧法、差示扫描量热法（DSC）、热重分析（TG）法等方法测试了阻燃粘胶纤维的燃烧性能和热稳定性。随着阻燃剂含量的增加，其阻燃效果明显增强，含16%阻燃剂的阻燃粘胶纤维LOI值为28.5%，接火3次以上，燃烧失重率为21.12%，属于难燃纤维，经30次水洗测试仍保持阻燃效果。阻燃剂的加入使粘胶纤维的第一次分解温度提前约20℃，分解速度加快；二次碳化时变得困难，第二次分解速度变缓，碳化温度滞后约30~50℃。纤维燃烧后表面生成碳化层，保留了纤维的结构。
首先采用共混法将蛋白液、阻燃剂与粘胶纺丝液共混制备出阻燃蛋白粘胶纤维。在阻燃剂添加量保持在16%的基础上再加入5%的动物蛋白，通过SEM观察发现制得的阻燃蛋白粘胶纤维内部结构更加紧密，纤维表面出现了均匀散状分布的小孔；经LOI及45度燃烧测试，30次水洗前后的阻燃蛋白粘胶纤维均能达到难燃纤维标准。性能测试表明，阻燃蛋白粘胶纤维的主要改善是取向度、机械强度明显提高，回潮率比普通粘胶纤维略差，但较阻燃粘胶纤维的回潮率大13.3%，保温性有所提高；摩擦系数较阻燃粘胶纤维要小；膨松度提高，并超过普通粘胶纤维；在后加工过程中通过改性氨基有机硅柔软剂进行表面改性得到了具有丝滑手感的纤维。
采用表面抗菌整理的方法将壳聚糖及纳米银-壳聚糖复合抗菌整理液应用到阻燃蛋白粘胶纤维中。处理后的抗菌阻燃蛋白粘胶纤维对混合菌的抑菌率分别达92.4%和97.6%，水洗30次后仍能达到89.3%和93.8%。纤维水洗前后LOI值均保持在29%以上，通过氮元素含量的测定发现了阻燃效果叠加规律；抗菌整理后的纤维干强比抗菌整理前有所提高，比普通粘胶纤维低，湿强则较普通粘胶纤维高；摩擦系数较抗菌整理前增大；通过改性氨基有机硅柔软剂的柔软整理，使最终制备的纤维摩擦系数低于普通粘胶纤维的摩擦系数，使最终样品的阻燃性能、机械强度、服用性能、抗菌性能都达到最优。
The demands of quantity and quality of flame-retardant textiles increasedramatically with the rapid development of technology and the booming consumptionlevel. In viscose fiber industry, environemental-firendly flame retardants are required, aswell as excellent wearing performance and antibacterial property. However,multi-functional product with combined features has not been reported. In this paper,flame-retardant viscose fiber was prepared by the addition of an environment-friendlyphosphazene derivative, hexaphenoxycyclotriphosphazene (HPTP). Flame-retardantprotein viscose fiber was prepared by adding animal protein solution to spinning solution.By using chitosan as antibacterial agent, Antibacterial flame-retardant protein viscosefiber was prepared for the first time. Flame retardancy, mechanical strength, wearingperformance and other properties of these viscose fibers were studied systematically.
In this paper, HPTP was applied to the study of flame-retardant viscose fiber for thefirst time. Sodium phenate and hexachlorocyclotriphosphazene (HCTP) were used asreactants to synthesize HPTP. Reaction factors such as temperature, time and reactantratio were optimized using orthogonal test design, which gave a yield of76.52%. A yieldof97.3%was accomplished after PEG400was added as catalyst. Infrared spectrum and31P NMR spectrum were employed to characterize and determine the structure of theproduct. Results showed that Cl atoms were replaced completely. Differential scanningcalorimetry (DSC) and Thermogravimetry (TG) results indicated that the decompositiontemperature of HPTP is250degree centigrade higher than that of HCTP. It proved thatHPTP is a flame retardant with better heat-resistance.
APG/EL-20emulsification system was selected and optimized using orthogonal testdesign to solve the bad dissolubility of HPTP before wet spinning. HPTP was blendedwith viscose spinning solution thoroughly. Fluffy structures spread uniformly wereobserved on the cross section of flame-retardant viscose fiber. The igniting property andthermal stability of the samples were evaluated by scanning electron microscope (SEM),Limited oxygen index (LOI),45degree igniting test, DSC, TG. The results indicated thathigher flame retardant percentage fiber has better flame retardancy. Viscose fiber with 16%flame retardant was evaluated as flame-retardant fiber (LOI=28.5%, ignition time>3, ignition weight loss=21.12%). The flame retardancy of the fiber remained after30times wash test. The first decomposition temperature of flame-retardant viscose fiber wasdecreased by20degree centigrade, decomposition rate was accelerated. Secondarycarbonization was more difficult than beforedecomposition rate was slower and the peakof decomposition was lagged by30~50degree centigrade. After igniting test, carbonizedlayer was formed on the surface of flame-retardant viscose fiber, the structure of fiberremained. Mechanical strength of the fiber with our emulsification system performedbetter than viscose fiber with common emulsification system.
Protein solution, flame retardant and viscose spinning solution were blended for thefirst time to prepare flame-retardant protein viscose fiber. Animal protein was added5%by weight to spinning solution on the basis of16%flame retardant. The product has morecompact structure inside the fiber and evenly scattered small pores on the surface. Resultsof LOI and45degree igniting test showed that the flame-retardant protein viscose fibercan reach the flame-retardant standard both before and after30times wash test. The chiefimprovement of this product is the better orientation and mechanical strength. Moistureregain of the fiber is a little lower than that of normal viscose fiber, however, it is13.3%higher than the moisture regain of flame-retardant viscose fiber, heat retention is alsoimproved. Friction coefficient of the product is lower than that of flame-retardant viscosefiber. Bulking intensity is increased, better than that of normal viscose fiber. The productwas modified with modified amino organic silicon softener to obtain silk-like feel.
Chitosan and Ag nanoparticles-chitosan antibacterial agent were used to finish theflame-retardant protein viscose fiber. After modification the antibacterial flame-retardantprotein viscose fiber showed92.4%and97.6%inhibition to mixed strain,89.3%and93.8%after30times wash teat, respectively. LOI of the product is higher than29%before and after wash test. The improvement of the flame retardanc is based on theaccumulation of N element. Dry mechanical strength of the fiber is increased while stilllower than normal viscose fiber. However, the wet mechanical strength is much improvedthan that of normal viscose fiber. Friction coefficient is increased. After modification byusing modified amino organic silicon softener, the friction coefficient is lower than that of normal viscose fiber. The final product has optimized flame retardancy, mechanicalstrength, wearing performance and antibacterial function.
引文
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