复合氧化物纳米粉体颜料的制备和表征

Synthesis and Characterization of Mixed Metal Oxide Pigments

印染行业重点技术发展的目标之一就是研制开发高效、环保、安全的新型染化料,为了解决纺织印染中的废水污染问题,发展无水印染新技术,是一个引起人们广泛关注的新研究方向。我们受红宝石,蓝宝石结构特征的启发,尝试采用均相沉淀法合成以α-氧化铝为基质,通过少量掺杂呈色离子的复合氧化物颜料。实验中,将结晶氯化铝和一定比例的发色离子氯化物混合,用适量的蒸馏水溶解,再溶入尿素和聚乙烯吡咯烷酮,超声振荡均匀,将上述液体加热回流,煅烧反应后的产物,得到纳米无机颜料。通过XRD测定样品的晶型和纯度,确定新型颜料的主体成分是α-氧化铝,用紫外可见光谱仪测试样品的漫反射光谱,发现掺杂离子周围的配位环境变化导致吸收峰谱带发生变化。在此基础上用分光密度仪表征样品的色度,应用SEM进行微观形貌分析,样品粒径范围在200～300nm。将制成的复合氧化物颜料用饱和盐酸浸泡,对浸出液进行ICP测试,发现掺杂离子溶出量非常少,说明新型颜料具有良好的化学稳定性。上述结果说明,这类新型无机纳米粉体颜料各种耐性良好、无毒害,可以满足熔体纺丝要求,有望在无水印染方面得到应用。

In the present work,aluminum chloride and various soluble salts of doping ions were dissolved in water.In addition,urea and polyvinyl pyrrolidone（PVP） were also dissolved in the above aqueous solution under supersonic treatments.Then the solutions were heated to induce the hydrolysis of urea so that soluble aluminum and doping ions convert into insoluble hydroxide or carbonate gels.After calcinations,the obtained gels change to mixed metal oxide pigments whose color is related to type and concentrations of the doping ions.XRD characterization demonstrates that the diffraction patterns of the products are the same as that of α-alumina.Diffuse reflectance spectra of samples of the samples in UV-Vis regions show that the absorption bands for d—d transitions of the doping ions undergo considerable change as the coordinate environments change.In addition,L＊,a＊ and b＊ values of the pigments were measured by using UV-Vis densitometer.SEM results indicate that the size of the pigment powders is in the range 200～300 nm.The pigments are quite stable since no evidence of dissolution was observed after the synthesized pigment is soaked for 24 hours.ICP test shows that very little amount of doped metal occurs in the corresponding filtrate.The above results suggest that these new kinds of mixed metal oxide pigments are stable,non-toxic,environmental friendly and they may be applicable in molten spinning process and provide a new chance for non-aqueous printing and dyeing industry.