天然染料超临界CO_2萃取染色一步法技术研究
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摘要
超临界CO_2具有良好的溶解扩散性能，使得其可代替水作为染色介质，由于它具有节能、节水、工艺流程短等特点，已成为国内外染整行业的研究热点。目前，对超临界染色技术的研究仅限于使用化学染料的阶段，为实现天然纤维的良好染色效果，人们不得不使用各种改性方法，以增加染料与纤维之间的亲和性。这种研究的负面影响是：一方面增加了成本；另一方面，使得原本绿色环保的超临界染色工艺，在改性时产生污染。为了开发无污染、低能耗的“生态绿色”生产工艺，本文采用天然姜黄为染料，在超临界CO_2染色装置中完成萃取—染色一步法工艺。
论文阐述了超临界CO_2的性质、热力学原理和传质机理，提出了超临界CO_2萃取—染色一步法工艺技术，建立了天然姜黄收缩核模型，从分子水平分析了天然姜黄素的晶体结构以及姜黄素与天然纤维的结合性能。由于姜黄素的分子较小，分子极性小，在超临界CO_2中溶解度较大，可得到较好的分散性能，实现了萃取—染色一步法。
采用正交试验和单因素试验分析的方法，对天然纤维织物和化学纤维织物进行超临界CO_2萃取—染色一步法实验。对超临界萃取染色工艺对染色颜色特征值的影响进行了研究，确定了最优染色条件。结果表明：在萃取染色一步法工艺中，姜黄粒度(φ)大小影响甚大，随粒度减小，色差增大、得色增深、固着率增加，姜黄粒度为0.5mm色差和固着率均最大；采用内染、外染结合的工艺，可提高织物匀染性，缩短染色时间；染色效果化学纤维优于蛋白质纤维和纤维素纤维，缠绕织物染色形式优于层放织物。毛织物最优工艺为：姜黄粒度φ=0.5mm、27Mpa、80℃、50min；棉织物最优工艺为：姜黄粒度φ=0.5mm、27Mpa、100℃、50min；PET织物最优工艺为：姜黄粒度φ=0.5mm、27Mpa、80℃、50min。
超临界CO_2萃取染色一步法工艺具有上染时间短、织物匀染性好、色牢度优的特点，为天然染料应用于超临界CO_2染色工艺技术的研究提供了理论基础。
The fine performance of supercfitical CO_2 on dissolution and diffusion make it substitutefor water as dyeing medium. As a result of its characteristic such as the conservation of energyand water and the short technical process, the research of supercritical CO_2 dyeing technologyhas become a hot spot in domestic and foreign dyeing and finishing industry. Currently, theresearch of supereritical CO_2 dyeing technology was restricted in the application stage ofchemical dyestuffs. Kinds of finishing methods have to be utilized to make natural fibersachieve the good dyeing effect, by dint of the improvement of compatibility between dyestuffsand fibers. However, the negative influence of this kind of research is: on the one hand,finishing increases the costs; the other, supercfitical dyeing process is originally green, butpollution may be caused by finishing. To the development of "eco-green" technology withnon-pollution and low-energy-consumption, the curcuma is adopted as dye in this paper, and theone step extracting-dyeing technology has been carried out in supercritical CO_2 dyeinginstrument.
The nature, thermodynamic principles and mass transfer mechanism of the supercfiticalCO_2 are elaborated. The one step extracting-dyeing technology in supercritical CO_2 has beenproposed. The shrinking core model of natural curcuma is established. The crystal structure andbinding characteristic with natural fibers of natural curcumin are analyzed from the molecularlevel. The curcumin obtains good performance of solubility and dispersibility in supercriticalCO_2, because its molecule size and molecule polarity is both small. Therefore the one stepextracting-dyeing technology has been achieved.
The the one step extracting-dyeing technology in supercritical CO_2 experiments aredesigned and implemented on natural fiber fabrics and chemical fiber fabrics throughorthogonal experiments and single factor experiments. The optimal dyeing parameters havebeen determined by the study of the influence of supercfitical CO_2 extracting-dyeing craft ondyeing-color eigenvalues. The results indicate that, in extracting-dyeing one-stage craft, theparticle size of eurcuma is an important influencing factor. The chromatic aberration, hue and fixing rate increased along with the reducing of particle size of curcuma. The maximum valuesof the chromatic aberration and fixing rate are obtained when the particle size of curcuma is0.5mm. The level dyeing property is improved and the dyeing time is reduced by applying theassociative craft of inside dyeing and outside dyeing. The dyeing effect of chemical fibers isbetter than that of protein fibers and cellulose fibers, and the dyeing form of winding fabricsurpasses that of stacking. The optimal dyeing craft for wool fabric is as follows: the diameterof the curcuma particle is 0.5mm, the pressure is 27MPa, the temperature is 80℃and thedyeing time is 50min. The optimal dying craft for cotton fabric is that 0.5mm, 27MPa, 100℃and 50min. The optimal dying craft for PET fabric is that 0.5mm, 27MPa, 80℃and 50min.
The the one step extracting-dyeing technology in supercfitical CO_2 has many superiorcharacteristic, such as short dyeing time and excellent levelness and color fastness. Therationale has been provided for applying the natural dyestuff to the supercritical CO_2 dyeingcraft technology research.
论文阐述了超临界CO_2的性质、热力学原理和传质机理，提出了超临界CO_2萃取—染色一步法工艺技术，建立了天然姜黄收缩核模型，从分子水平分析了天然姜黄素的晶体结构以及姜黄素与天然纤维的结合性能。由于姜黄素的分子较小，分子极性小，在超临界CO_2中溶解度较大，可得到较好的分散性能，实现了萃取—染色一步法。
采用正交试验和单因素试验分析的方法，对天然纤维织物和化学纤维织物进行超临界CO_2萃取—染色一步法实验。对超临界萃取染色工艺对染色颜色特征值的影响进行了研究，确定了最优染色条件。结果表明：在萃取染色一步法工艺中，姜黄粒度(φ)大小影响甚大，随粒度减小，色差增大、得色增深、固着率增加，姜黄粒度为0.5mm色差和固着率均最大；采用内染、外染结合的工艺，可提高织物匀染性，缩短染色时间；染色效果化学纤维优于蛋白质纤维和纤维素纤维，缠绕织物染色形式优于层放织物。毛织物最优工艺为：姜黄粒度φ=0.5mm、27Mpa、80℃、50min；棉织物最优工艺为：姜黄粒度φ=0.5mm、27Mpa、100℃、50min；PET织物最优工艺为：姜黄粒度φ=0.5mm、27Mpa、80℃、50min。
超临界CO_2萃取染色一步法工艺具有上染时间短、织物匀染性好、色牢度优的特点，为天然染料应用于超临界CO_2染色工艺技术的研究提供了理论基础。
The fine performance of supercfitical CO_2 on dissolution and diffusion make it substitutefor water as dyeing medium. As a result of its characteristic such as the conservation of energyand water and the short technical process, the research of supercritical CO_2 dyeing technologyhas become a hot spot in domestic and foreign dyeing and finishing industry. Currently, theresearch of supereritical CO_2 dyeing technology was restricted in the application stage ofchemical dyestuffs. Kinds of finishing methods have to be utilized to make natural fibersachieve the good dyeing effect, by dint of the improvement of compatibility between dyestuffsand fibers. However, the negative influence of this kind of research is: on the one hand,finishing increases the costs; the other, supercfitical dyeing process is originally green, butpollution may be caused by finishing. To the development of "eco-green" technology withnon-pollution and low-energy-consumption, the curcuma is adopted as dye in this paper, and theone step extracting-dyeing technology has been carried out in supercritical CO_2 dyeinginstrument.
The nature, thermodynamic principles and mass transfer mechanism of the supercfiticalCO_2 are elaborated. The one step extracting-dyeing technology in supercritical CO_2 has beenproposed. The shrinking core model of natural curcuma is established. The crystal structure andbinding characteristic with natural fibers of natural curcumin are analyzed from the molecularlevel. The curcumin obtains good performance of solubility and dispersibility in supercriticalCO_2, because its molecule size and molecule polarity is both small. Therefore the one stepextracting-dyeing technology has been achieved.
The the one step extracting-dyeing technology in supercritical CO_2 experiments aredesigned and implemented on natural fiber fabrics and chemical fiber fabrics throughorthogonal experiments and single factor experiments. The optimal dyeing parameters havebeen determined by the study of the influence of supercfitical CO_2 extracting-dyeing craft ondyeing-color eigenvalues. The results indicate that, in extracting-dyeing one-stage craft, theparticle size of eurcuma is an important influencing factor. The chromatic aberration, hue and fixing rate increased along with the reducing of particle size of curcuma. The maximum valuesof the chromatic aberration and fixing rate are obtained when the particle size of curcuma is0.5mm. The level dyeing property is improved and the dyeing time is reduced by applying theassociative craft of inside dyeing and outside dyeing. The dyeing effect of chemical fibers isbetter than that of protein fibers and cellulose fibers, and the dyeing form of winding fabricsurpasses that of stacking. The optimal dyeing craft for wool fabric is as follows: the diameterof the curcuma particle is 0.5mm, the pressure is 27MPa, the temperature is 80℃and thedyeing time is 50min. The optimal dying craft for cotton fabric is that 0.5mm, 27MPa, 100℃and 50min. The optimal dying craft for PET fabric is that 0.5mm, 27MPa, 80℃and 50min.
The the one step extracting-dyeing technology in supercfitical CO_2 has many superiorcharacteristic, such as short dyeing time and excellent levelness and color fastness. Therationale has been provided for applying the natural dyestuff to the supercritical CO_2 dyeingcraft technology research.
引文
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