工业钛液水解制备窄粒径偏钛酸产品工艺优化及调控机制
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作者单位:

1.攀枝花学院 钒钛学院,四川 攀枝花 617000 ;2.钒钛关键战略材料四川省重点实验室,四川 攀枝花 617000

作者简介:

吴越(2000—),女,四川乐至人,硕士研究生在读,主要从事功能性二氧化钛等的研究。

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中图分类号:

TF823;TF125

基金项目:

四川省科技计划项目(2025ZNSFSC0379,2024ZHCG0141);攀枝花市科技计划项目(25KJJH0025);攀枝花学院研究生创新计划项目(y2025021)


Process optimization and control mechanism of narrow particle size metatitanic acid prepared by hydrolysis of industrial titanyl sulfate solution
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Affiliation:

1.School of Vanadium and Titanium, Panzhihua University, Panzhihua 617000 , China ;2.Vanadium and Titanium Critical Strategic Materials Key Laboratory of Sichuan Province, Panzhihua 617000 , China

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    摘要:

    针对我国硫酸法钛白粉普遍存在粒径分布宽、高端产能匮乏的现状,本研究以低浓度工业钛液为原料,采用自生晶种水解工艺,系统探究了底水量、钛液 TiO2浓度和熟化时间对偏钛酸粒径分布的内在调控机制,并通过表征结果分析其与最终颗粒尺寸、结构形貌之间的构效关系,得到以下主要结论。 最优水解工艺参数为底水量16%、钛液浓度205 g/L、熟化时间25 min,此条件下,制备出的偏钛酸产品径距比低至 1.01,属于窄粒径分布,且工艺稳定性优异。水解所制的偏钛酸是由(30~60) nm的晶粒通过晶界堆积而成的类球形多晶聚集体,由于水解初期阴离子(SO4 2- 、OH- )在晶核表面的吸附,产生的空间位阻效应与静电斥力阻碍了晶核向单晶演化,促使其通过团聚形成表面富含羟基与结合水的介孔水合胶体结构。粒径调控基于“成核-生长-团聚”多阶段的竞争耦合,底水量通过调节初始过饱和度降低成核势垒,确立成核优势;TiO2浓度通过调节体系黏度增加传质阻力,抑制晶粒粗化与硬团聚;熟化时间通过调控水解速率,有效抑制奥斯瓦尔德熟化效应导致的粒径宽化。本研究结果可为工业制备高性能钛白粉提供优质原料生产参数与工艺参考。

    Abstract:

    In view of the current situation of wide particle size distribution and lack of high-end production capacity of titanium dioxide by sulfuric acid method in China, in this study, low-concentration industrial titanyl sulfate solution was used as raw material, and authigenic seed hydrolysis process was used to systematically explore the internal regulation mechanism of bottom water volume, titanium liquid TiO2 concentration and curing time on the particle size distribution of metatitanic acid. The structure-activity relationship between the final particle size and structure morphology was analyzed by the characterization results, and the following main conclusions were obtained. The optimal hydrolysis process parameters were as follows: bottom water 16%, titanium solution concentration 205 g/L, and curing time 25 min. Under these conditions, the diameter-to-distance ratio of the prepared metatitanic acid product was as low as 1. 01, which belonged to a narrow particle size distribution and had excellent process stability. The metatitanic acid prepared by hydrolysis is a spherical polycrystalline aggregate formed by the accumulation of (30-60) nm grains through grain boundaries. Due to the adsorption of anions (SO4 2- , OH- ) on the surface of the crystal nucleus at the initial stage of hydrolysis, the steric hindrance effect and electrostatic repulsion generated hinder the evolution of the crystal nucleus to single crystal, which promotes the formation of a mesoporous hydrated colloidal. The particle size control is based on the multi-stage competitive coupling of 'nucleation-growth-agglomeration'. The bottom water volume reduces the nucleation barrier by adjusting the initial supersaturation and establishes the nucleation advantage. The concentration of TiO2 increases the mass transfer resistance by adjusting the viscosity of the system, and inhibits grain coarsening and hard agglomeration. The ripening time effectively inhibits the particle size broadening caused by the Ostwald ripening effect by regulating the hydrolysis rate. The results can provide production parameters and process reference for industrial preparation of high-performance titanium dioxide.

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吴越,杜肖阳,王青鸿,等. 工业钛液水解制备窄粒径偏钛酸产品工艺优化及调控机制[J]. 中国有色冶金,2026,55 (1):1-7.

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  • 收稿日期:2025-11-18
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  • 在线发布日期: 2026-03-27
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