分散染料微胶囊制备及应用研究
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摘要
近年来，由于工业的迅猛发展和人口膨胀，水的消耗急剧增加。众所周知，纺织工业中印染生产工序产生大量的染色废水对水质和环境造成严重的危害。纺织行业面临的主要挑战是：不增加成本，保证产品质量，同时解决环境问题。
本论文以纯分散染料为芯材和蜜胺预聚体为壁材采用原位聚合法制备分散染料微胶囊，借助差热分析(DSC)、扫描电镜(SEM)、粒径分布仪表征分散染料微胶囊的外观特征、耐热性能、平均粒径及粒径分布；采用微胶囊技术对涤纶和尼龙进行分散染料清洁染色研究。采用分散染料微胶囊对锦纶织物进行无助剂染色；利用不同颜色的分散染料微胶囊对超细涤纶织物进行无助剂染色，探索染色废水经简单过滤后循环用于织物煮练和染色的可能性。通过测色配色仪评价织物色泽和染色均匀性；利用制备的微胶囊分散红60、微胶囊分散黄54和微胶囊分散蓝56对聚酯膜进行动力学研究。
主要结果归纳如下：
(1)以纯分散染料为芯材，蜜胺预聚体为壁材利用原位聚合法制备微胶囊。研究制备微胶囊影响因素：芯壁比、剪切速率、溶液pn值、乳化剂用量和壁材滴加时间。制备分散染料微胶囊最佳剪切速率为不低于10000min~(-1)，溶液的pH值宜为3-4，壁材滴加时间不低于2.5小时，乳化剂用量为(2-3)％。
(2)实验以1：1芯壁比的C.I.分散蓝56微胶囊为对象，通过分散染料微胶囊对锦纶染色研究发现，分散染料微胶囊宜在较高温度下才能达到商品染料的色深，如在100℃下，分散染料微胶囊不仅可以提高锦纶染色的高温匀染性、移染性，而且微胶囊染色对pH值依存性较小，分散染料微胶囊完全可以替代商品染料对锦纶进行均匀染色，且分散染料微胶囊染色无需添加助剂，其染色后废水经简单处理，可实现循环再染色。此外，染色样品在不含胶囊的染浴中处理一段时间之后，即可免除水洗而达到良好的牢度。
(3)利用1：3芯壁比的C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊对涤纶在130℃下进行上染试验，三色上染曲线一致性较好；采用芯壁比为1：3的C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊对涤纶拼色，采用芯壁比为1：1的C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊对锦纶拼色，染制的色织物水洗牢度令人满意，说明C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊可以作为三原色微胶囊染料对锦纶或涤纶进行拼色。
(4)研究了C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊三种微胶囊化分散染料在聚酯薄膜中的扩散行为，并与传统的商品分散染料及无助剂的纯分散染料在聚酯薄膜中的扩散作了对比。结果表明：对于所有分散染料而言，随着温度的升高，扩散系数D均增加，但与商品分散染料相比，微胶囊分散染料的扩散系数及无助剂的纯分散染料的扩散系数均较小。由不同温度下的扩散系数计算出扩散活化能E，表面活性剂的存在使商品染料的扩散活化能有所降低。
(5)分别以C.I.分散蓝291、C.I.分散紫93、C.I.分散橙288三种分散染料作为芯材，通过原位聚合法制备分散染料微胶囊，然后三种颜色微胶囊按一定比例相混合，复配成微胶囊分散黑。利用制备的分散染料微胶囊分别对超细纤维织物在常规高温染色设备中进行，研究其染色废水再循环用于染色和前处理，实验表明，染色废水经简单过滤后可以循环再利用；同时采用分散黑微胶囊与常规商品染料黑进行比较，色织物各项性能指标均优异，说明采用分散黑微胶囊替代商品染料黑进行高温高压超细纤维染色可以达到废水再循环利用。
分散染料微胶囊对锦纶和涤纶进行无助剂染色研究揭示：分散染料微胶囊完全可以替代商品染料对涤纶、锦纶进行均匀染色，且分散染料微胶囊染色无需添加助剂，其染色后废水经简单处理，可实现循环再利用。此外，染色样品在不含胶囊的染浴中处理一段时间之后，即可免除水洗而达到良好的牢度，获得经济效益和环境效益的双重效果。
The volume of water consumed by human beings has increased dramatically in recentyears while water supply remains constant. Both of population growth and the expansion ofindustrial activity require more water consumption. It is well known that the dyeing andprinting processes in textile industry produce large amounts of waste water which causesserious problem to water quality and the environment. The main challenge that textileindustries faces is to keep the balance between solving the environmental problems andinsuring the product quality while keeping general cost low.
In this study, microencapsulation technique was applied by using melamine prepolymeras wall material in order to achieve the clean dyeing of disperse dye onto PET or Nylon fabrics.Melamine resin microcapsules containing pure disperse dye were prepared by in situpolymerization. Differential scanning calorimetry (DSC), scanning electron microcopy(SEM)and particle size analyzer were used to obtain information about the characters of themicrocapsules on structure, morphologies, a mean particle size and size distribution. Thedyeing behaviors of microencapsulated disperse dyes were evaluated on polyamide fabrics inabsence of auxiliaries. A series of microencapsulated disperse dyes in different color wereprepared for super-micro polyester fabrics dyeing without dispersant addition. The possibilityof recycling microencapsulated disperse dyes bath effluent for secondary dyeing and scouringafter simple filtration was assessed, and the results were compared to those using distilledwater. The spectral reflectance value and relative levelness of each sample were collectedusing a Datacolor Spectraflash 600. Dyeing kinetics of PET membrane were studied withdisperse dye C.I. Disperse Red 60, disperse dye C.I. Disperse Yellow 54 and disperse dye C.I.Disperse Blue 56.
The main results are summarized as following:
(1) Microcapsules were prepared by in situ with pure disperse dye as the core material andmelamine prepolymer as the wall-former. The influence of core-to-wall ratio, the stirring rate,pH value of the solution,the dosage of emulsifier and dropping time of wall material werediscussed. The results showed that the optimum conditions for preparing microencapsulateddisperse dye were defined as sheafing rate higher than 10000rpm, suitable pH value 3-5,dropping time over 2 hours and the dosage of emulsifier 2%-3%.
(2) According to the dyeing of polyamide fabric with microcapsule disperse dyes(C:W=1:1), it was found that dyeing with microcapsule disperse dyes should be carried out at a little bithigher temperature, so that the same depth of dyeing as that of the corresponding commercialdisperse dyes can be achieved. For example, dyeing polyamide fabric with microcapsuledisperse dye at 100℃can not only enhance the high temperature levelness and migration, butalso reduce its dependence on pH value. So, it can be surely used as a substitute for thecommercial dye in polyamide fabric dyeing, and has such advantages as no need of addingdyeing assistants, and recyclable use of dyeing effluent after simply filtered. In addition, thedyeings after only treated in the dye-bath containing no microcapsules for a certain timefeatured good color fastness without rinsing or washing.
(3) Dyeing processes were carried out with microencapsuled dyestuffs of C.I. disperse red 60,C.I. disperse yellow 54 and C.I. disperse blue 56 with the ratio of core to wall 1:3,whichshowed that three dyeing Curves had good compatibility. The combination of three dyestuffswith the ratio, of core to wall 1:3 and 1:1 were used to dye polyester or polyamide fabrics andthe dyeings all featured good color fastness to washing.
(4) Diffusion behaviors of microcapsules containing disperse dyestuffs, such asmicroencapsuled dyestuffs of C.I. disperse red 60, microencapsuled dyestuffs of C.I. disperseyellow 54 and microencapsuled dyestuffs of C.I. disperse blue 56 in polyester film werestudied, and the results were compared with those of commercial disperse dyestuffs and theirpure types. It was shown that for all the disperse dyes, the diffusion coefficient D wouldincrease along with the increase of temperature. The diffusion activation energy E calculatedfrom D under different temperatures showed that the existence of surfactants would lead to thedecrease in diffusion activation energy.
(5) Microcapsules were prepared with C.I. disperse blue 291, C.I. disperse violet 93 and C.I.orange 288 individually, and these three microcapsules were combined in a certain proportionto dye supermicro polyester fabric in conventional high-temperature dyeing machine. Thedyeing effluent treated by simple filtration was recycled for dyeing and scouring. Acceptablechanges in color and dark-white difference were assessed. All the dyeings featured goodlevelness and fastness to washing, rubbing and light fastness. Microencapsuled disperse dyescan be surely used in dyeing super-micro polyester fabrics without surfactants, and theeffluents can be recycled. Being thoroughly auxiliary free, using microencapsuled dispersedyes dyeing method costs much less in eliminating pollution than using traditional method.
It can be surely used as a substitute for the commercial dye in dyeing polyester andpolyamide fabric and has such advantages as no need of adding dyeing assistants, andrecyclable use of the effluent only after simple filtration. In addition, the dyeings treated in thedye-bath containing no microcapsules for a certain time, possessed good color fastnesswithout rinsing or washing, which was beneficial for environmental protection.
本论文以纯分散染料为芯材和蜜胺预聚体为壁材采用原位聚合法制备分散染料微胶囊，借助差热分析(DSC)、扫描电镜(SEM)、粒径分布仪表征分散染料微胶囊的外观特征、耐热性能、平均粒径及粒径分布；采用微胶囊技术对涤纶和尼龙进行分散染料清洁染色研究。采用分散染料微胶囊对锦纶织物进行无助剂染色；利用不同颜色的分散染料微胶囊对超细涤纶织物进行无助剂染色，探索染色废水经简单过滤后循环用于织物煮练和染色的可能性。通过测色配色仪评价织物色泽和染色均匀性；利用制备的微胶囊分散红60、微胶囊分散黄54和微胶囊分散蓝56对聚酯膜进行动力学研究。
主要结果归纳如下：
(1)以纯分散染料为芯材，蜜胺预聚体为壁材利用原位聚合法制备微胶囊。研究制备微胶囊影响因素：芯壁比、剪切速率、溶液pn值、乳化剂用量和壁材滴加时间。制备分散染料微胶囊最佳剪切速率为不低于10000min~(-1)，溶液的pH值宜为3-4，壁材滴加时间不低于2.5小时，乳化剂用量为(2-3)％。
(2)实验以1：1芯壁比的C.I.分散蓝56微胶囊为对象，通过分散染料微胶囊对锦纶染色研究发现，分散染料微胶囊宜在较高温度下才能达到商品染料的色深，如在100℃下，分散染料微胶囊不仅可以提高锦纶染色的高温匀染性、移染性，而且微胶囊染色对pH值依存性较小，分散染料微胶囊完全可以替代商品染料对锦纶进行均匀染色，且分散染料微胶囊染色无需添加助剂，其染色后废水经简单处理，可实现循环再染色。此外，染色样品在不含胶囊的染浴中处理一段时间之后，即可免除水洗而达到良好的牢度。
(3)利用1：3芯壁比的C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊对涤纶在130℃下进行上染试验，三色上染曲线一致性较好；采用芯壁比为1：3的C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊对涤纶拼色，采用芯壁比为1：1的C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊对锦纶拼色，染制的色织物水洗牢度令人满意，说明C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊可以作为三原色微胶囊染料对锦纶或涤纶进行拼色。
(4)研究了C.I.分散红60微胶囊、C.I.分散黄54微胶囊、C.I.分散蓝56微胶囊三种微胶囊化分散染料在聚酯薄膜中的扩散行为，并与传统的商品分散染料及无助剂的纯分散染料在聚酯薄膜中的扩散作了对比。结果表明：对于所有分散染料而言，随着温度的升高，扩散系数D均增加，但与商品分散染料相比，微胶囊分散染料的扩散系数及无助剂的纯分散染料的扩散系数均较小。由不同温度下的扩散系数计算出扩散活化能E，表面活性剂的存在使商品染料的扩散活化能有所降低。
(5)分别以C.I.分散蓝291、C.I.分散紫93、C.I.分散橙288三种分散染料作为芯材，通过原位聚合法制备分散染料微胶囊，然后三种颜色微胶囊按一定比例相混合，复配成微胶囊分散黑。利用制备的分散染料微胶囊分别对超细纤维织物在常规高温染色设备中进行，研究其染色废水再循环用于染色和前处理，实验表明，染色废水经简单过滤后可以循环再利用；同时采用分散黑微胶囊与常规商品染料黑进行比较，色织物各项性能指标均优异，说明采用分散黑微胶囊替代商品染料黑进行高温高压超细纤维染色可以达到废水再循环利用。
分散染料微胶囊对锦纶和涤纶进行无助剂染色研究揭示：分散染料微胶囊完全可以替代商品染料对涤纶、锦纶进行均匀染色，且分散染料微胶囊染色无需添加助剂，其染色后废水经简单处理，可实现循环再利用。此外，染色样品在不含胶囊的染浴中处理一段时间之后，即可免除水洗而达到良好的牢度，获得经济效益和环境效益的双重效果。
The volume of water consumed by human beings has increased dramatically in recentyears while water supply remains constant. Both of population growth and the expansion ofindustrial activity require more water consumption. It is well known that the dyeing andprinting processes in textile industry produce large amounts of waste water which causesserious problem to water quality and the environment. The main challenge that textileindustries faces is to keep the balance between solving the environmental problems andinsuring the product quality while keeping general cost low.
In this study, microencapsulation technique was applied by using melamine prepolymeras wall material in order to achieve the clean dyeing of disperse dye onto PET or Nylon fabrics.Melamine resin microcapsules containing pure disperse dye were prepared by in situpolymerization. Differential scanning calorimetry (DSC), scanning electron microcopy(SEM)and particle size analyzer were used to obtain information about the characters of themicrocapsules on structure, morphologies, a mean particle size and size distribution. Thedyeing behaviors of microencapsulated disperse dyes were evaluated on polyamide fabrics inabsence of auxiliaries. A series of microencapsulated disperse dyes in different color wereprepared for super-micro polyester fabrics dyeing without dispersant addition. The possibilityof recycling microencapsulated disperse dyes bath effluent for secondary dyeing and scouringafter simple filtration was assessed, and the results were compared to those using distilledwater. The spectral reflectance value and relative levelness of each sample were collectedusing a Datacolor Spectraflash 600. Dyeing kinetics of PET membrane were studied withdisperse dye C.I. Disperse Red 60, disperse dye C.I. Disperse Yellow 54 and disperse dye C.I.Disperse Blue 56.
The main results are summarized as following:
(1) Microcapsules were prepared by in situ with pure disperse dye as the core material andmelamine prepolymer as the wall-former. The influence of core-to-wall ratio, the stirring rate,pH value of the solution,the dosage of emulsifier and dropping time of wall material werediscussed. The results showed that the optimum conditions for preparing microencapsulateddisperse dye were defined as sheafing rate higher than 10000rpm, suitable pH value 3-5,dropping time over 2 hours and the dosage of emulsifier 2%-3%.
(2) According to the dyeing of polyamide fabric with microcapsule disperse dyes(C:W=1:1), it was found that dyeing with microcapsule disperse dyes should be carried out at a little bithigher temperature, so that the same depth of dyeing as that of the corresponding commercialdisperse dyes can be achieved. For example, dyeing polyamide fabric with microcapsuledisperse dye at 100℃can not only enhance the high temperature levelness and migration, butalso reduce its dependence on pH value. So, it can be surely used as a substitute for thecommercial dye in polyamide fabric dyeing, and has such advantages as no need of addingdyeing assistants, and recyclable use of dyeing effluent after simply filtered. In addition, thedyeings after only treated in the dye-bath containing no microcapsules for a certain timefeatured good color fastness without rinsing or washing.
(3) Dyeing processes were carried out with microencapsuled dyestuffs of C.I. disperse red 60,C.I. disperse yellow 54 and C.I. disperse blue 56 with the ratio of core to wall 1:3,whichshowed that three dyeing Curves had good compatibility. The combination of three dyestuffswith the ratio, of core to wall 1:3 and 1:1 were used to dye polyester or polyamide fabrics andthe dyeings all featured good color fastness to washing.
(4) Diffusion behaviors of microcapsules containing disperse dyestuffs, such asmicroencapsuled dyestuffs of C.I. disperse red 60, microencapsuled dyestuffs of C.I. disperseyellow 54 and microencapsuled dyestuffs of C.I. disperse blue 56 in polyester film werestudied, and the results were compared with those of commercial disperse dyestuffs and theirpure types. It was shown that for all the disperse dyes, the diffusion coefficient D wouldincrease along with the increase of temperature. The diffusion activation energy E calculatedfrom D under different temperatures showed that the existence of surfactants would lead to thedecrease in diffusion activation energy.
(5) Microcapsules were prepared with C.I. disperse blue 291, C.I. disperse violet 93 and C.I.orange 288 individually, and these three microcapsules were combined in a certain proportionto dye supermicro polyester fabric in conventional high-temperature dyeing machine. Thedyeing effluent treated by simple filtration was recycled for dyeing and scouring. Acceptablechanges in color and dark-white difference were assessed. All the dyeings featured goodlevelness and fastness to washing, rubbing and light fastness. Microencapsuled disperse dyescan be surely used in dyeing super-micro polyester fabrics without surfactants, and theeffluents can be recycled. Being thoroughly auxiliary free, using microencapsuled dispersedyes dyeing method costs much less in eliminating pollution than using traditional method.
It can be surely used as a substitute for the commercial dye in dyeing polyester andpolyamide fabric and has such advantages as no need of adding dyeing assistants, andrecyclable use of the effluent only after simple filtration. In addition, the dyeings treated in thedye-bath containing no microcapsules for a certain time, possessed good color fastnesswithout rinsing or washing, which was beneficial for environmental protection.
引文
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