光致变色微胶囊的制备及其应用研究
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摘要
光致变色材料在印刷、防伪、包装,尤其是国防工业等方面有着广泛的应用前景。有机光致变色材料具有变色灵敏、色泽鲜艳的特点,但易受温度、光照、pH值和氧等环境因素的影响而导致氧化劣变,耐疲劳性差,影响了它在纺织品领域的应用。
本文以含有光致变色材料螺噁嗪的四氯乙烯溶液为芯材、蜜胺树脂为壁材、SDS为乳化剂、PVA为分散剂,采用原位聚合技术制备了光致变色微胶囊,并将其应用于纺织品中,制备光致变色织物。实验研究了光致变色溶液浓度对其变色性能的影响,甲醛/三聚氰胺摩尔比对微胶囊表面形貌及强度的影响;乳化速度、乳化时间、乳化剂的浓度、分散剂的浓度、酸化时间等条件对光致变色微胶囊表面形貌及粒径分布的影响;探讨了壁材/芯材体积用量比及乳化设备对光致变色微胶囊密封性及变色情况的影响。利用光学显微镜、扫描电子显微镜(SEM)、热重分析仪(TGA)、激光粒度仪等仪器对光致变色微胶囊的性能进行表征。通过计算,得出光致变色微胶囊的囊壁厚度。采用乙酰丙酮法检测了光致变色微胶囊中游离甲醛的含量,并对制备的光致变色织物的耐皂洗牢度和摩擦牢度进行测试。
研究结果表明,当变色溶液浓度为0.75%时,获得最好的变色效果;甲醛/三聚氰胺的摩尔比为3/1、搅拌速度为1000rpm、乳化时间为40min、酸化时间0.5h、乳化剂浓度为0.5%、分散剂浓度为0.2%、壁材/芯材体积比4/1时,制得的光致变色微胶囊在日光照射下显示紫色,并能实现快速可逆显色反应;光致变色微胶囊中的游离甲醛含量为35～142mg/kg ,符合GB18401-2001规定的甲醛含量限定标准。
将高速乳化机制备的光致变色微胶囊涂覆到针织物表面,获得在日光下能够快速可逆变色的光致变色织物,该织物具有良好的耐皂洗牢度和摩擦牢度。
Photochromic materials have extensive application prospect in printing, security, packaging, particularly the defense industry. The organic photochromic materials with sensitive color changing and bright color were susceptible to be affected by temperature, light, pH value, oxygen and other enviromental factors, which led to oxidation and deterioration and poor fatigue resistance. And these enviromental factors impact its application in the field of textile.
In this paper, photochromic microcapsules were prepared via in-situ polymerization, and perchlorethylene solution of spiroozaxine, melamine resin, SDS, PVA were used as core materials, wall materials, emulsifier and dispersant. The effects of photochromic solution concentration on color changing property and formaldehyde/melamine molar ratio on surface morphology and intensity of microcapsule were studied. Moreover, the influencing surface morphology and size distribution of the photochromic microcapsules, such as mixing speed, emulsifying time, emulsifier and dispersant concentration and acidification timewere discussed in detail. The effects of volume ratio of wall materials/core materials and emulsifier equipment to sealing and color changing of photochromic microcapsule were argued. The properties of photochromic microcapsules were analyzed by Optical Microscope, Scanning Electron Microscopy, Thermal Gravimetric Analysis, Laser Particle Size Analyzer. The wall thickness of the photochromic microcapsule were calculated. The free formaldehyde content of the photochromic microcapsules were detected through acetylacetone method. The soaping fastness and resistance rubbing fastness of photochromic fabric were tested.
The results had shown that the best effect of color changing was obtained when the photochromic solution concentration was 0.75wt%. When the molar ratio of formaldehyde to melamine is 3/1, the rate of emulsifier is 1000rpm, the emulsifier time is 40 min, the acidification time is 0.5h, the emulsifier concentration is 0.5wt%, the dispersant concentration is 0.2wt%, the volume ratio of wall materials to core materials is 4/1, the photochromic microcapsules showing purple irradiated under sunlight were obtained. And these microcapsules could rapid and reversible change color. The free formaldehyde detecting results had conformed that the free formaldehyde of microcapsules in this paper ranged the GB18401-2001 standard limit.
The photochromic microcapsules prepared using high-speed emulsification machine were coated on the surface of knitting-needle fabric. The photochromic fabrics was gained and could be rapid reversible changing color under sunlight. And this fabric had better resistance soaping fastness and rubbing fastness.
本文以含有光致变色材料螺噁嗪的四氯乙烯溶液为芯材、蜜胺树脂为壁材、SDS为乳化剂、PVA为分散剂,采用原位聚合技术制备了光致变色微胶囊,并将其应用于纺织品中,制备光致变色织物。实验研究了光致变色溶液浓度对其变色性能的影响,甲醛/三聚氰胺摩尔比对微胶囊表面形貌及强度的影响;乳化速度、乳化时间、乳化剂的浓度、分散剂的浓度、酸化时间等条件对光致变色微胶囊表面形貌及粒径分布的影响;探讨了壁材/芯材体积用量比及乳化设备对光致变色微胶囊密封性及变色情况的影响。利用光学显微镜、扫描电子显微镜(SEM)、热重分析仪(TGA)、激光粒度仪等仪器对光致变色微胶囊的性能进行表征。通过计算,得出光致变色微胶囊的囊壁厚度。采用乙酰丙酮法检测了光致变色微胶囊中游离甲醛的含量,并对制备的光致变色织物的耐皂洗牢度和摩擦牢度进行测试。
研究结果表明,当变色溶液浓度为0.75%时,获得最好的变色效果;甲醛/三聚氰胺的摩尔比为3/1、搅拌速度为1000rpm、乳化时间为40min、酸化时间0.5h、乳化剂浓度为0.5%、分散剂浓度为0.2%、壁材/芯材体积比4/1时,制得的光致变色微胶囊在日光照射下显示紫色,并能实现快速可逆显色反应;光致变色微胶囊中的游离甲醛含量为35～142mg/kg ,符合GB18401-2001规定的甲醛含量限定标准。
将高速乳化机制备的光致变色微胶囊涂覆到针织物表面,获得在日光下能够快速可逆变色的光致变色织物,该织物具有良好的耐皂洗牢度和摩擦牢度。
Photochromic materials have extensive application prospect in printing, security, packaging, particularly the defense industry. The organic photochromic materials with sensitive color changing and bright color were susceptible to be affected by temperature, light, pH value, oxygen and other enviromental factors, which led to oxidation and deterioration and poor fatigue resistance. And these enviromental factors impact its application in the field of textile.
In this paper, photochromic microcapsules were prepared via in-situ polymerization, and perchlorethylene solution of spiroozaxine, melamine resin, SDS, PVA were used as core materials, wall materials, emulsifier and dispersant. The effects of photochromic solution concentration on color changing property and formaldehyde/melamine molar ratio on surface morphology and intensity of microcapsule were studied. Moreover, the influencing surface morphology and size distribution of the photochromic microcapsules, such as mixing speed, emulsifying time, emulsifier and dispersant concentration and acidification timewere discussed in detail. The effects of volume ratio of wall materials/core materials and emulsifier equipment to sealing and color changing of photochromic microcapsule were argued. The properties of photochromic microcapsules were analyzed by Optical Microscope, Scanning Electron Microscopy, Thermal Gravimetric Analysis, Laser Particle Size Analyzer. The wall thickness of the photochromic microcapsule were calculated. The free formaldehyde content of the photochromic microcapsules were detected through acetylacetone method. The soaping fastness and resistance rubbing fastness of photochromic fabric were tested.
The results had shown that the best effect of color changing was obtained when the photochromic solution concentration was 0.75wt%. When the molar ratio of formaldehyde to melamine is 3/1, the rate of emulsifier is 1000rpm, the emulsifier time is 40 min, the acidification time is 0.5h, the emulsifier concentration is 0.5wt%, the dispersant concentration is 0.2wt%, the volume ratio of wall materials to core materials is 4/1, the photochromic microcapsules showing purple irradiated under sunlight were obtained. And these microcapsules could rapid and reversible change color. The free formaldehyde detecting results had conformed that the free formaldehyde of microcapsules in this paper ranged the GB18401-2001 standard limit.
The photochromic microcapsules prepared using high-speed emulsification machine were coated on the surface of knitting-needle fabric. The photochromic fabrics was gained and could be rapid reversible changing color under sunlight. And this fabric had better resistance soaping fastness and rubbing fastness.
引文
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