琥珀酰亚胺酯基类偶氮染料的制备及其超临界CO2羊毛清洁化染色

Preparation of Azo Dyes Based on Succinimide and Their Dyeing of Wool in Supercritical CO2

摘要:

以对氨基苯甲酸和4-氨基-2-氯苯甲酸、苯胺和间甲苯胺为原料，采用重氮偶合反应制备染料前驱体，通过在前驱体上引入琥珀酰亚胺酯获得4例活性分散染料Ⅰ~Ⅳ。对染料的吸收光谱、光热稳定性、超临界二氧化碳（scCO2）中羊毛纤维的染色工艺等进行了测试。结果表明，4例染料均具有良好的光热稳定性，且染料Ⅰ，Ⅲ和Ⅳ最大吸收波长集中在360~370 nm，染料Ⅱ的最大吸收波长红移到400~450 nm，染料均具备scCO2染色的条件。染料Ⅰ和Ⅲ的最佳染色条件为2 h，80℃和15 MPa，染料Ⅱ的最佳染色条件为1.5 h，80℃和15 MPa，染料Ⅳ的最佳染色条件为1.5 h，80℃和24 MPa。染色后的羊毛纤维的耐皂洗和耐光色牢度都可达4~5级，固色率最高可达86%，相比于未活化的前驱体，耐皂洗色牢度能提高2~3级，固色率最高能提升63%。SEM和显微镜成像较好地证明了4例染料具有良好的透染性，且能均匀附着于纤维的表面和内部。力学性能测试表明，染色后的羊毛纤维能基本保持原有的力学性能。

Abstract:

Four kinds of reactive disperse dyes Ⅰ~Ⅳ were prepared by the diazo coupling reaction in which succinimide ester was introduced into precursors. The data of absorption spectrum, photo-thermal stability, process of supercritical carbon dioxide (scCO2) dyeing wool fibers were tested. The results show that four dyes have good photo-thermal stability, and the maximum absorption wavelengths for dyes Ⅰ, Ⅲ and Ⅳ are observed at the range of 360-370 nm, and the maximum absorption wavelength for dye II has a red shift to 400-450 nm. Thus, the dyes are suitable for scCO2 dyeing. The optimal dyeing conditions for dyes are as follows: 2 h, 80 ℃ and 15 MPa for Ⅰ and Ⅲ, 1.5 h, 80℃ and 15 MPa for dye Ⅱ, and 1.5 h, 80 ℃ and 24 MPa for dye Ⅳ. The soaping fastness to soaping and light of the dyed wool fibers can reach 4-5 grade, and the fixation rate can reach up to 86%. Compared with un-activated precursor, the color fastness to soaping improves 2~3 grades, and the fixation rate increases 63%. Scanning electron microscopy (SEM) and microscopy images show that four dyes have good dyes’ permeability, evenly adhere to the surface and interior of the fibers. The test of mechanical parameters shows that the dyed wool fibers can basically maintain the original mechanical properties.