纳米炭黑的Steglich酯化反应制备及乙二醇分散性  

Preparation of carbon black nanoparticles by Steglich esterification and its ethylene glycol dispersity

作　　者：王玉玺 唐春霞 张丽平 付少海[1,2] WANG Yuxi;TANG Chunxia;ZHANG Liping;FU Shaohai(Jiangsu Engineering Research Center for Digital Textile Inkjet Printing,Wuxi,Jiangsu 214122,China;Key Laboratory of Eco-Textiles(Jiangnan University),Ministry of Education,Wuxi,Jiangsu 214122,China)

机构地区：[1]江苏省纺织品数字喷墨印花工程技术研究中心,江苏无锡214122 [2]生态纺织教育部重点实验室(江南大学),江苏无锡214122

出　　处：《纺织学报》2024年第7期104-111,共8页Journal of Textile Research

基　　金：国家自然科学基金面上项目(22278185)。

摘　　要：为解决炭黑在乙二醇溶液中难分散的问题,确保炭黑在聚酯纤维原液着色中具有良好的分散性。先通过液相氧化法对炭黑表面进行改性,在炭黑表面引入反应性基团—羧基,并选取合适的氧化炭黑,通过Steglich酯化反应在氧化炭黑表面接枝乙二醇和不同相对分子质量的聚乙二醇。对氧化炭黑和接枝炭黑的表面结构以及在乙二醇溶液中的分散性进行测试与分析。结果表明:氧化仅发生在炭黑表面并未对炭黑造成严重破坏,随氧化时间的延长,炭黑表面羧基含量显著提高,氧化8 h后,其表面羧基含量为0.616 mmol/g;PEG600接枝的氧化炭黑其接枝率在33%以上,最小平均粒径稳定在132.1 nm左右,其能在乙二醇溶液中分散均匀,无聚集体出现,且制备的接枝炭黑具有良好的分散稳定性,其储存稳定性在93%以上,耐热稳定性在92%以上。Objective Among polyester fibers,the black polyester fibers are in great demand.The black polyester fiber produced by conventional printing and dyeing methods is found to have poor color fastness and produce a large amount of printing and dyeing wastewater,but the black polyester produced by dope dyeing can avoid these problems.However,strong mechanical aggregates are formed between the carbon black pigment particles in ethylene glycol-based color paste,and it is difficult to obtain a stable and good glycol-based carbon black pigment suspension and dispersion system.Therefore,it is necessary to modify the carbon black to solve the problem of poor dispersion during the coloring of polyester fiber stock solution.Method Liquid phase oxidation method was adopted to oxidize carbon black with nitric acid for different time durations(2,4,6,8 h),and the oxidized carbon black was then characterized by X-ray photoelectron spectroscopy,X-ray diffraction,and other instruments to screen out suitable oxidized carbon black.In the presence of dicyclohexylcarbodiimide and 4-dimethylaminopyridine,the 4 h oxidized carbon black was adopted to perform Steglich esterification reaction with ethylene glycol(EG),polyethylene glycol 200(PEG200),polyethylene glycol 600(PEG600)and pollyethylene glycol 800(PEG800)in N,N-dimethylformamide to prepare grafted carbon black,which were named EG-OCB,PEG200-OCB,PEG600-OCB,PEG800-OCB,respectively.according to the graft polymers.The grafted carbon black was analyzed and tested.Results Through nitric acid oxidation,the particle size of the original carbon black was reduced from 6686 nm to 156.5-174.9 nm,and the particle size of the carbon black was the smallest with 4 h oxidation.Subsequently,the surface of oxidized carbon black was grafted,and the particle size was further reduced under steric hindrance effect.Compared with the original carbon black,the particle dispersion of oxidized carbon black and grafted carbon black was obvious,and no large aggregates appeared.The oxygen-containing functional gr

关 键 词：纳米炭黑 氧化 分散性 聚酯纤维原液着色 酯化接枝 聚乙二醇 Steglich酯化反应 

分 类 号：TS193[轻工技术与工程—纺织化学与染整工程]