A special magenta dye SCFX-AYRL with dichlorotriazine as reactive group, designed as one of supercritical trichromatic dyes, was successfully synthesized for sustainable coloration of natural fibers in supercritical fluid of carbon dioxide (SCF-CO 2 ). The products were characterized and tested by FT-IR, 1 H NMR, LC-MS, EA and Uv-Vis spectra. Moreover, Gaussian software was also employed to assist a theoretical design of the dye and its precursor, such as the optimization of structure conformations, the calculation of frontier molecular orbitals and parameters, and the prediction of characteristic absorption wavelength. The obtained results show that the molecular structure and color characteristics of the synthesized dye well met the expected theoretical design and calculations. Particularly, the powerfully excited molecular orbitals facilitated the first electron transition from the highest occupied orbital (HOMO) to the lowest unoccupied molecular orbital (LUMO) by contributing characteristic singlet absorption bands for the precursor and its target dye. Moreover, an energy gap (Δ E ) calculation between the LUMO and the HOMO was performed to predict color hue shift, and was well consistent with experimental detects. A successful application of the special dye on natural protein fibers was observed for eco-friendly coloration in SCF-CO 2 with high color strength, fixation efficiency over 90.0 %, as well as high brilliant color and fastness.
Fan Wang,Meng-Yue Li,Shu-Jing Long,Yuan-Bin Zheng,Xin-Xin Cao,Zi-Qing Du,An-Tong Liu,Jia-Jie Long
An efficient and ecofriendly method to remove impurities from raw cashmere fiber was constructed by employing various biological enzymes ( lipase , cellulase , pectinase and protease ) to form reverse microemulsion in supercritical carbon dioxide. An investigation and optimization of various parameters, such as the dosage of biological enzymes, cleaning temperature, pressure and duration for this method were performed according to the whiteness and weight loss of the treated samples. Then the proposed method was further validated by energy dispersive X-ray spectrometry (EDS), scanning electron microscopy (SEM) analysis to verify the impurity removal from cashmere fiber. Moreover, the aggregation structure and properties of cleaned cashmere fiber were also investigated by X-ray powder diffraction (XRD), strength measurement, moisture absorption testing and thermal analysis (TG-DTG). The results declare that, via forming a type of (W+enzymes)/SCF-CO 2 microemulsion to transfer the biological enzymes into supercritical medium, various impurities from raw cashmere fiber could be efficiently decreased and removed, which cleaning performance was better than a conventional control process. The cleaning efficiency for various impurities was notably influenced by the dosages of the applied enzymes and system parameters, which could be improved at an appropriate condition in SCF-CO 2 . Furthermore, the cleaning feasibility, reliability and efficiency of the enzymatically catalyzed method for raw cashmere fiber was successfully verified by SEM, EDS, XRD, TG-DTG, tensile strength analysis, and a supercritical cleaning mechanism for raw cashmere was further proposed.
Developing new reactive disperse dyes and applying them to dye natural fiber substrates in the supercritical fluid of carbon dioxide (SCF–CO 2 ) is of great importance for ecological protection and the sustainable development of the textile industry. In this work, a reactive disperse dye with an anthraquinonoid chromogen in blue hue and a dichlorotriazine reactive group was successfully designed and synthesized. The precursor of the anthraquinonoid derivative reactive disperse dye was synthesized with a one-pot amination reaction method by employing the reactions between 1, 4-dihydroxyanthraquinone or its cryptochrome 1, 4-diaminoanthraquinone and aniline, ethylenediamine. Then, the precursor was subjected to continuously react with a reactive group of cyanuric chloride to obtain a dichlorotriazine type reactive disperse dye. Moreover, the chemical structures and color characteristics of the final dye, as well as the precursor, were characterized and confirmed by Fourier transform infrared spectroscopy (FT-IR), 1 H nuclear magnetic resonance ( 1 H NMR), and ultraviolet–visible absorption spectroscopy (UV–Vis). Additionally, the anthraquinonoid derivative reactive disperse dye was preliminarily applied to the coloration of cotton and wool substrates in SCF-CO 2 . The coloration results show that the staining fastness and the dry, wet rubbing fastness of the reactive disperse dye on both cotton and wool substrates were satisfactory.