茉莉香精微胶囊的制备及其在棉织物上的应用研究
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摘要
为了增加纺织品的附加值,近年来开发功能性纺织品的呼声越来越高。将功能性整理剂通过缓释微胶囊包覆可以实现织物的多种长效功能整理如驱虫、芳香、抗菌、润肤等以及将具有医学作用的抗生素、荷尔蒙等应用在纺织品上从而成为具有医疗效果的服装材料。微胶囊技术的原理是将易挥发的活性物质包裹在微型容器内从而使活性物质以缓慢的速度释放。通过印花、浸轧、浸染、涂层等方式,借助于粘合剂可以将微胶囊牢固地附着在纤维上,从而提高功能织物的耐久性。
现代研究表明茉莉花香对失眠、焦虑、烦躁等症状有良好的缓解作用。传统药物虽然效果明显,却容易使服用者上瘾且会引起抑郁、眩晕、低血压、协调能力受损等副作用,茉莉香气能缓解焦虑、促进睡眠,比传统药物更适合于医疗保健,但其易挥发的特性既使之味道过于浓郁也使得功效难以持久。
本文采用原位聚合法以蜜胺树脂为壁材,茉莉香精为芯材,对双层造壁缓释性微胶囊的制备及其缓释性能进行了详细的研究,并借助热焙烘技术及紫外光固化技术将其应用在织物上,研究制备出具有较好耐久性的茉莉芳香织物。论文主要由三个部分组成：(1)茉莉香精微胶囊的制备,详细分析了芯壁比、预聚体滴加速度对微胶囊外观形貌以及热稳定性的影响,探讨了降低香精微胶囊游离甲醛的方法,确定了适用于织物芳香整理的香精微胶囊的制备工艺；(2)使用水性聚氨酯粘合剂和聚丙烯酸粘合剂将香精微胶囊整理到织物上,研究了粘合剂的种类以及焙烘条件对芳香织物耐水洗性能的影响,得出最佳处理工艺并研究了芳香织物的耐摩性能及物理机械性能的变化；(3)使用水基紫外光固化粘合剂将香精微胶囊应用在织物上,研究了整理方式、光引发剂的种类、光源的种类、光固化的时间对芳香织物耐水洗性能的影响,得出了最佳的处理工艺并研究了芳香织物的自然留香性能及物理机械性能。运用FTIR及ATR-FTIR表征茉莉香精微胶囊的包埋情况及紫外光固化粘合剂的固化情况；借助光学显微镜及热分析仪观察微胶囊的形态及分析微胶囊的热稳定性能；使用激光粒度仪测定了微胶囊的平均粒径及粒径分布；利用主观评价和客观分析相结合的方法表征织物的香味；通过SEM观察芳香织物的外观形态。主要结果归纳如下：
(1)茉莉香精、蜜胺树脂、微胶囊的OM及FTIR图谱显示茉莉香精成功地被蜜胺树脂包埋。在一定的预聚体滴加速度下,降低芯壁比有利于提高微胶囊的热稳定性能,但无助于改善微胶囊的形貌；通过降低预聚体的滴加速度,不仅提高了微胶囊的热稳定性能也改善了其形貌。微胶囊制备结束后使用双氧水、尿素、过硫酸铵等都可以降低微胶囊的游离甲醛,但尿素更适合用作香精微胶囊的去游离甲醛处理。制备微胶囊的最佳工艺条件为芯壁比1：1,预聚体滴加速度0.6mL/min,反应结束后加入足量的尿素可除去游离甲醛。
(2)采用热固化粘合剂通过浸轧-焙烘的方式将微胶囊应用在棉织物上,主观评价和客观分析的结果表明聚氨酯粘合剂处理的芳香织物的耐水洗次数在5次左右,聚丙烯酸粘合剂处理的芳香织物耐水洗次数达到了15次,提高焙烘条件可以增加芳香织物的耐水洗次数。使用聚氨酯粘合剂进行芳香整理时的最佳焙烘条件为150℃下处理2min,使用聚丙烯酸类粘合剂时的最佳焙烘条件为160℃下处理2min,经过聚氨酯粘合剂或者聚丙烯酸粘合剂处理的芳香织物可以经受6,000次的摩擦。聚丙烯酸粘合剂处理的织物的断裂强力、硬挺度均高于聚氨酯粘合剂,聚氨酯粘合剂处理的织物的白度总体上稍高于聚丙烯酸粘合剂,两者的游离甲醛含量达到了内衣游离甲醛的释放标准。
(3)采用紫外光固化粘合剂将香精微胶囊应用在棉织物上,研究结果表明采取合适的整理方式,选用合适的光引发剂、紫外光源,使用一定量的光引发剂及一定的固化时间可以显著提高芳香织物的耐水洗性能。当使用涂层整理方式,采用20 g/kg的光引发剂Runtecure1265,在1000W的有极高压汞灯下固化4min时,芳香织物的耐水洗能力达到30次,整理后的芳香织物断裂强力增加了约3.7%,硬挺度增加了约40.7%,白度下降为42左右,织物的游离甲醛含量低于内衣游离甲醛的释放标准。
Nowadays, developing new products with high added-value properties is very imperative for the textile industry. Encapsulation techniques allow an opportunity for the application of some functional agents on fabrics, such as insect repellents, anti-cellulite treatments, long-lasting fragrances, skin softeners and some medical applications such as antibiotics, hormones and other drugs. This innovative technology makes use of microcapsules which act as small containers of liquids to be released from the inner core under controlled conditions to address a specific purpose. The microcapsules can be applied on textiles by printing, exhaustion dyeing, impregnation and coating. A binder agent is required for the combination of microcapsules in the fabrics, its function is to fix the microcapsules in the fabric to improve the durability.
According to some researches released recently, jasmine scent, like tranquilizer is helpful to the alleviation of insomnia, anxiety and fidget. The traditional medicines can give rise to addicting and even lead to some side-effects despite of its effectiveness in curing, however jasmine scent doesn't have such drawbacks.
In this paper, a control-release jasmine microcapsules were synthesized using melamine resin and jasmine essential oils by in-situ polymeriztion. Fragrant fabrics with good durabilities were prepared using thermal curable binders and UV curable binders respectively. The whole study was composed of three parts:(1) In the preparation of jasmine microcapsules, effect of ratio of core and shell ratio and droping rate of melamine resin prepolymers on the microcapsules morphology and thermal stabilities, methods of reducing the remnant free formaldehyde were carried out. An appropriate preparation method of preparation of jasmine microcapsules was established. (2) using polyurethane binder and acrylic binder to prepare fragrant cotton fabrics. The effect of different kinds of binders and different thermal curing conditions on the washing durability were discussed. A fit finishing method was established and physical properties and abrasion test were conducted. (3) using water-based UV curable binder to fix microcapsules on cotton fabrics. Effects of finishing method, photoinitiators, UV light lamps, curing time on the washing durability of fragrant fabrics were investigated. A premium finishing method was also established and physical properties were tested. The structure of the microcapsules and fragrant fabrics were characterized by the FTIR and ATR-FTIR, the morphology characteristics of the microcapsules and fragrant fabrics were observed by means of optical microscopy and SEM,the particle size and size distribution of the microcapsules were measured by the laser particle analyzer. Odor evaluation was carried out by human olfactory sensations and ultraviolet absorption spectrophotometry. The main results were summarized as follows:
(1) FTIR spectra of jasmine oil, melamine resin, jasmine microcapsules showed that jasmine oil had been microencapsulated by melamine resin. Under certain dropping rates of melamine resin prepolymer, reducing the ratio of core and shell helps to increase the thermal stability of microcapsules, however worsen the morphology the microcapsules. Slowing down the ratio of core and shell can help to improve the morphology while maintaining good thermal stability. After the reaction, hydrogen peroxide, urea, ammonium persulfate can be used to eliminate the remnant free formaldehyde, and urea seems to be the most suitable one. The optimum conditions for jasmine microcapsule preparation were defined as 1:1 ratio of core and shell, dropping rate of melamine resin prepolymer 0.6mL/min, and urea as anti-formaldehyde agent.
(2) By using thermal curable binders, the jasmine microcapsules were fixed onto the cotton fabric by dipping padding method. The results showed that polyurethane binder can make fragrant fabric endure 5 washing cycles, acrylic binder can make fragrant fabric bear 15 washing cycles. The stronger the curing condition, the higher the washing durability of finished samples. The optimum curing condition for polyurethane and acrylic binder were 150℃for 2min and 160℃for 2min respectively. The finished fabrics could bear over 6,000 abrasion cycles and the physical properties didn't change significantly. Acrylic binder treated fragrant fabric had higher breaking strength and stiffness than polyurethane binder, while polyurethane binder treated fragrant fabric had a higher white index than acrylic binder. The free formaldehyde content could reach the underwear standard.
(3) By using UV curable binder, jasmine microcapsules were novelly applied on the cotton fabric. The results showed that finishing method, photoinitiator and UV light lamp can have great influence on the washing durability of the fragrant fabric. When using coating method,20g/kg Runtecure1265 as photoinitiator,1000W electrode high pressure mercury arc continuous UV light as UV light source, curing for 4min, the fragrant fabric could bear 30 washing cycles. The breaking strength and stiffness of the finished fabric increased about 3.7% and 40.7% respectively, white index reduced to 42. Free formaldehyde content met the underwear standard.
现代研究表明茉莉花香对失眠、焦虑、烦躁等症状有良好的缓解作用。传统药物虽然效果明显,却容易使服用者上瘾且会引起抑郁、眩晕、低血压、协调能力受损等副作用,茉莉香气能缓解焦虑、促进睡眠,比传统药物更适合于医疗保健,但其易挥发的特性既使之味道过于浓郁也使得功效难以持久。
本文采用原位聚合法以蜜胺树脂为壁材,茉莉香精为芯材,对双层造壁缓释性微胶囊的制备及其缓释性能进行了详细的研究,并借助热焙烘技术及紫外光固化技术将其应用在织物上,研究制备出具有较好耐久性的茉莉芳香织物。论文主要由三个部分组成：(1)茉莉香精微胶囊的制备,详细分析了芯壁比、预聚体滴加速度对微胶囊外观形貌以及热稳定性的影响,探讨了降低香精微胶囊游离甲醛的方法,确定了适用于织物芳香整理的香精微胶囊的制备工艺；(2)使用水性聚氨酯粘合剂和聚丙烯酸粘合剂将香精微胶囊整理到织物上,研究了粘合剂的种类以及焙烘条件对芳香织物耐水洗性能的影响,得出最佳处理工艺并研究了芳香织物的耐摩性能及物理机械性能的变化；(3)使用水基紫外光固化粘合剂将香精微胶囊应用在织物上,研究了整理方式、光引发剂的种类、光源的种类、光固化的时间对芳香织物耐水洗性能的影响,得出了最佳的处理工艺并研究了芳香织物的自然留香性能及物理机械性能。运用FTIR及ATR-FTIR表征茉莉香精微胶囊的包埋情况及紫外光固化粘合剂的固化情况；借助光学显微镜及热分析仪观察微胶囊的形态及分析微胶囊的热稳定性能；使用激光粒度仪测定了微胶囊的平均粒径及粒径分布；利用主观评价和客观分析相结合的方法表征织物的香味；通过SEM观察芳香织物的外观形态。主要结果归纳如下：
(1)茉莉香精、蜜胺树脂、微胶囊的OM及FTIR图谱显示茉莉香精成功地被蜜胺树脂包埋。在一定的预聚体滴加速度下,降低芯壁比有利于提高微胶囊的热稳定性能,但无助于改善微胶囊的形貌；通过降低预聚体的滴加速度,不仅提高了微胶囊的热稳定性能也改善了其形貌。微胶囊制备结束后使用双氧水、尿素、过硫酸铵等都可以降低微胶囊的游离甲醛,但尿素更适合用作香精微胶囊的去游离甲醛处理。制备微胶囊的最佳工艺条件为芯壁比1：1,预聚体滴加速度0.6mL/min,反应结束后加入足量的尿素可除去游离甲醛。
(2)采用热固化粘合剂通过浸轧-焙烘的方式将微胶囊应用在棉织物上,主观评价和客观分析的结果表明聚氨酯粘合剂处理的芳香织物的耐水洗次数在5次左右,聚丙烯酸粘合剂处理的芳香织物耐水洗次数达到了15次,提高焙烘条件可以增加芳香织物的耐水洗次数。使用聚氨酯粘合剂进行芳香整理时的最佳焙烘条件为150℃下处理2min,使用聚丙烯酸类粘合剂时的最佳焙烘条件为160℃下处理2min,经过聚氨酯粘合剂或者聚丙烯酸粘合剂处理的芳香织物可以经受6,000次的摩擦。聚丙烯酸粘合剂处理的织物的断裂强力、硬挺度均高于聚氨酯粘合剂,聚氨酯粘合剂处理的织物的白度总体上稍高于聚丙烯酸粘合剂,两者的游离甲醛含量达到了内衣游离甲醛的释放标准。
(3)采用紫外光固化粘合剂将香精微胶囊应用在棉织物上,研究结果表明采取合适的整理方式,选用合适的光引发剂、紫外光源,使用一定量的光引发剂及一定的固化时间可以显著提高芳香织物的耐水洗性能。当使用涂层整理方式,采用20 g/kg的光引发剂Runtecure1265,在1000W的有极高压汞灯下固化4min时,芳香织物的耐水洗能力达到30次,整理后的芳香织物断裂强力增加了约3.7%,硬挺度增加了约40.7%,白度下降为42左右,织物的游离甲醛含量低于内衣游离甲醛的释放标准。
Nowadays, developing new products with high added-value properties is very imperative for the textile industry. Encapsulation techniques allow an opportunity for the application of some functional agents on fabrics, such as insect repellents, anti-cellulite treatments, long-lasting fragrances, skin softeners and some medical applications such as antibiotics, hormones and other drugs. This innovative technology makes use of microcapsules which act as small containers of liquids to be released from the inner core under controlled conditions to address a specific purpose. The microcapsules can be applied on textiles by printing, exhaustion dyeing, impregnation and coating. A binder agent is required for the combination of microcapsules in the fabrics, its function is to fix the microcapsules in the fabric to improve the durability.
According to some researches released recently, jasmine scent, like tranquilizer is helpful to the alleviation of insomnia, anxiety and fidget. The traditional medicines can give rise to addicting and even lead to some side-effects despite of its effectiveness in curing, however jasmine scent doesn't have such drawbacks.
In this paper, a control-release jasmine microcapsules were synthesized using melamine resin and jasmine essential oils by in-situ polymeriztion. Fragrant fabrics with good durabilities were prepared using thermal curable binders and UV curable binders respectively. The whole study was composed of three parts:(1) In the preparation of jasmine microcapsules, effect of ratio of core and shell ratio and droping rate of melamine resin prepolymers on the microcapsules morphology and thermal stabilities, methods of reducing the remnant free formaldehyde were carried out. An appropriate preparation method of preparation of jasmine microcapsules was established. (2) using polyurethane binder and acrylic binder to prepare fragrant cotton fabrics. The effect of different kinds of binders and different thermal curing conditions on the washing durability were discussed. A fit finishing method was established and physical properties and abrasion test were conducted. (3) using water-based UV curable binder to fix microcapsules on cotton fabrics. Effects of finishing method, photoinitiators, UV light lamps, curing time on the washing durability of fragrant fabrics were investigated. A premium finishing method was also established and physical properties were tested. The structure of the microcapsules and fragrant fabrics were characterized by the FTIR and ATR-FTIR, the morphology characteristics of the microcapsules and fragrant fabrics were observed by means of optical microscopy and SEM,the particle size and size distribution of the microcapsules were measured by the laser particle analyzer. Odor evaluation was carried out by human olfactory sensations and ultraviolet absorption spectrophotometry. The main results were summarized as follows:
(1) FTIR spectra of jasmine oil, melamine resin, jasmine microcapsules showed that jasmine oil had been microencapsulated by melamine resin. Under certain dropping rates of melamine resin prepolymer, reducing the ratio of core and shell helps to increase the thermal stability of microcapsules, however worsen the morphology the microcapsules. Slowing down the ratio of core and shell can help to improve the morphology while maintaining good thermal stability. After the reaction, hydrogen peroxide, urea, ammonium persulfate can be used to eliminate the remnant free formaldehyde, and urea seems to be the most suitable one. The optimum conditions for jasmine microcapsule preparation were defined as 1:1 ratio of core and shell, dropping rate of melamine resin prepolymer 0.6mL/min, and urea as anti-formaldehyde agent.
(2) By using thermal curable binders, the jasmine microcapsules were fixed onto the cotton fabric by dipping padding method. The results showed that polyurethane binder can make fragrant fabric endure 5 washing cycles, acrylic binder can make fragrant fabric bear 15 washing cycles. The stronger the curing condition, the higher the washing durability of finished samples. The optimum curing condition for polyurethane and acrylic binder were 150℃for 2min and 160℃for 2min respectively. The finished fabrics could bear over 6,000 abrasion cycles and the physical properties didn't change significantly. Acrylic binder treated fragrant fabric had higher breaking strength and stiffness than polyurethane binder, while polyurethane binder treated fragrant fabric had a higher white index than acrylic binder. The free formaldehyde content could reach the underwear standard.
(3) By using UV curable binder, jasmine microcapsules were novelly applied on the cotton fabric. The results showed that finishing method, photoinitiator and UV light lamp can have great influence on the washing durability of the fragrant fabric. When using coating method,20g/kg Runtecure1265 as photoinitiator,1000W electrode high pressure mercury arc continuous UV light as UV light source, curing for 4min, the fragrant fabric could bear 30 washing cycles. The breaking strength and stiffness of the finished fabric increased about 3.7% and 40.7% respectively, white index reduced to 42. Free formaldehyde content met the underwear standard.
引文
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