氟金云母钛珠光颜料的制备及表征

Preparation and Characterization of Fluorophlogopite Titania Pearlescent Pigment

利用硫酸沸腾水解法制备了氟金云母钛珠光颜料前驱体,并通过差热-热重分析确定了珠光颜料前驱体的煅烧工艺。通过正交实验考察了反应温度、初始pH值、反应时间、搅拌速度、钛液浓度、晶型促进剂(SnCl4)对前驱体包覆率的影响,得到了制备珠光颜料前驱体的最佳工艺条件以及影响包覆率的各因素的主次顺序。借助SEM、XRD、FT-IR以及EDS对煅烧前后的粉体进行了表征。测试结果表明:在优化的工艺条件下制得的珠光颜料表面致密光滑,包覆层为金红石型TiO2,包覆率为27.3%。

The fluorophlogopite titania pearlescent pigment precursor was prepared by boiling hydrolysis of TiCl4 solutions in dilute sulfuric acid at boiling state,and the calcining technology was identified by TG-DTA thermal analysis. The orthogonal experiment was used to get the optimal conditions of producing the precursor. The reaction temperature,initial pH,reaction time,mixing speed,the concentration of TiCl4,crystal accelerator （SnCl4） on precursor＇s coating rate were regarded as the influence factors in this orthogonal experiment. The optimal technology conditions to prepare the pigment precursor were gained. At the same time,the primary and secondary order of every factor which influences the coating rate of the precursor was confirmed. The powders were characterized by SEM,XRD,FT-IR and EDS. The results showed that under the optimal technology conditions,the surface of the pigment is dense and smooth without rift,the crystal of the coating layer is rutile and the coating rate of the pigment is 27.3%.