Synthesis of high purity TiO2 powders by fluidized gas hydrolysis

doi:10.11949/j.issn.0438-1157.20170515

Abstract

Abstract:

Synthesis of high purity TiO₂ powder by fluidized gas hydrolysis method is investigated.To tackle the problem of high Cl content remained in the TiO₂ powder,the hydrolysis reaction conditions and subsequently calcination at air,steam and H₂ are mainly investigated for dechlorination.The results show that the structure and phase transition of TiO₂ are two key factors that affect the efficiency of dechlorination.With the increase of the calcination temperature,the internal structure of TiO₂ is changed from porous to dense structure,and the crystalline structure is transformed from anatase to rutile.The structure and phase transition of TiO₂ are beneficial to increasing the removal rate of Cl.Compared with the air calcination,the dechlorination efficiency in water vapor atmosphere is obviously improved,which is attributed to the further reaction of water vapor and the multi hydroxyl chloride in the TiO₂ particles.Compared with air and steam calcination,the removal rate of Cl can be further improved up to 95% under the atmosphere of hydrogen at 800℃ for 2h,which is mainly attributed to the reduction of TiO₂ structure by hydrogen reduction.

Key words: fluidized-bed, hydrolysis, TiO₂, ultrafine powders, agglomeration

摘要：

针对TiCl₄气相水解制备TiO₂粉体存在Cl含量高的问题，开展了流化床TiCl₄气相水解制备高纯TiO₂。系统地研究了反应条件、煅烧后处理对TiO₂粉体的纯度、形貌、晶型、比表面积的影响。结果表明，TiO₂内部结构和晶型的转变有利于Cl的脱除；提高煅烧温度使TiO₂的内部结构由多孔疏松向致密结构转变，晶型结构由锐钛矿相向金红石相转变，从而有利于提高Cl的脱除率；与空气煅烧比较，水蒸气气氛下的脱氯效率明显提高，归因于水蒸气与TiO₂颗粒内残余的多羟基氯化物进一步反应；氢气气氛下可进一步提高Cl的脱除率，800℃煅烧2 h后Cl的脱除率达到95%，主要归因于氢气还原TiO₂使其晶型结构发生转变。

关键词: 流化床, 水解, 二氧化钛, 超细粉体, 团聚

CLC Number:

TQ031.5

ZHAO Yuzhong, SUN Jianjun, LI Jun, ZHU Qingshan. Synthesis of high purity TiO₂ powders by fluidized gas hydrolysis[J]. CIESC Journal, 2017, 68(10): 3978-3984.

赵玉仲, 孙建军, 李军, 朱庆山. 流化床气相水解制备高纯二氧化钛[J]. 化工学报, 2017, 68(10): 3978-3984.

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Synthesis of high purity TiO₂ powders by fluidized gas hydrolysis

流化床气相水解制备高纯二氧化钛

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