琥珀酰亚胺酯基类偶氮染料的制备及其超临界CO_(2)羊毛清洁化染色  

Preparation of azo dyes based on succinimide and their clean dyeing of wool in supercritical CO_(2)

作　　者：姚俊杰 侯俊 吕丽华[1] 贾孟珂 胡海娜 熊小庆[1,2] YAO Junjie;HOU Jun;LYU Lihua;JIA Mengke;HU Haina;XIONG Xiaoqing(Liaoning Provincial Key Laboratory of Textile Cleaning,Dalian Polytechnic University,Dalian 116034,Liaoning,China;State Key Laboratory of Fine Chemicals,Dalian University of Technology,Dalian 116024,Liaoning,China)

机构地区：[1]大连工业大学辽宁省清洁化纺织重点实验室,辽宁大连116034 [2]大连理工大学精细化工国家重点实验室,辽宁大连116024

出　　处：《精细化工》2021年第9期1920-1927,共8页Fine Chemicals

基　　金：国家自然科学基金(21606032);大连理工大学精细化工国家重点实验室开放课题基金资助项目(KF2013);大连市科技创新项目(2018J12GX056);大连市科技之星项目(2018RQ46)。

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。对染料的紫外-可见吸收光谱、光热稳定性、超临界二氧化碳(scCO_(2))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,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379~452 nm,染料均具备scCO_(2)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15MPa,染料Ⅳ的最佳染色条件为2 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和显微镜成像证明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。The dye precursors were prepared by diazo coupling reaction from p-aminobenzoic acid and 4-amino-2-chlorobenzoic acid, aniline and m-toluidine. Subsequently, four reactive disperse dyes Ⅰ~Ⅳ were obtained by introducing succinimide ester into the precursors. The UV-Vis spectra, photo-thermal stability of dyes and their dyeing process of wool fiber in supercritical carbon dioxide(scCO_(2)) were tested. The results showed that these dyes had good photo-thermal stability. The maximum absorption wavelengths of dyes Ⅰ, Ⅲ and Ⅳ were concentrated at 360~370 nm, and the maximum absorption wavelength of dye Ⅱ was redshifted to 379~452 nm, these dyes were suitable for scCO_(2) dyeing. The optimal dyeing conditions were as follows: 2 h, 80 ℃ and 15 MPa for dyes Ⅰ and Ⅲ;1.5 h, 80 ℃ and 15 MPa for dye Ⅱ;2 h, 80 ℃ and 24 MPa for dye Ⅳ. The color fastness to soaping and light of dyed wool fibers reached 4~5 grade, and the fixation rate could reach up to 86%, which were increased by 2~3 grade and 63% in comparison with that of un-activated precursor, respectively. The results of SEM and microscopy images indicated that four dyes possessed good permeability, and could uniformly attach to the surface and interior of the fibers. The mechanical properties of the dyed wool fibers were tested and the original mechanical properties were maintained after dyeing.

关 键 词：超临界二氧化碳染色 偶氮染料 活性染料 羊毛纤维 纺织染整助剂 

分 类 号：TQ630[化学工程—精细化工]