Chlorination of synthetic rutile with carbon tetrachloride at low temperature for producing titanium tetrachloride

FU Xiao; ZHANG Yinghao; WANG Yao; WEI Fei

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Chlorination of synthetic rutile with carbon tetrachloride at low temperature for producing titanium tetrachloride

更新时间：2025-12-10

- Chlorination of synthetic rutile with carbon tetrachloride at low temperature for producing titanium tetrachloride
- CIESC Journal Issue 12, Pages: 3026-3034(2009)
- 作者机构：
  
  清华大学化学工程系绿色反应工程与工艺北京市重点实验室,北京,100084
- 作者简介：
- 基金信息：
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  CLC：
- Online First：05 December 2009，
  
  Published：05 December 2009
- 稿件说明：
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FU Xiao, ZHANG Yinghao, WANG Yao, et al. Chlorination of synthetic rutile with carbon tetrachloride at low temperature for producing titanium tetrachloride[J]. CIESC Journal, 2009, (12): 3026-3034.
DOI：

FU Xiao, ZHANG Yinghao, WANG Yao, et al. Chlorination of synthetic rutile with carbon tetrachloride at low temperature for producing titanium tetrachloride[J]. CIESC Journal, 2009, (12): 3026-3034. DOI：

摘要

为了开发低温钛氯化工艺及解决工业副产物CCl4的再利用问题，在固定床和流化床反应器中考察了自贡法人造金红石原料与CCl4低温氯化制备TiCl4的反应过程，利用SEM、XRD、XPS等手段表征了人造金红石原料在反应前后的变化。结果显示，在450～500℃下，自贡法人造金红石能与CCl4快速反应生成TiCl4产品。少量Fe元素的掺杂是金红石相具备较高反应速率的关键原因。人造金红石原料制备过程中的弱氧化焙烧处理在颗粒表面形成的惰性金红石壳层，导致TiCl4收率极限为90%，但该壳层能在酸解过程以及低温CCl4氯化过程中维持颗粒粒度，使该原料能用于流化床操作。此过程具有显著的环保价值和工业应用前景。

Abstract

The chlorination of synthetic rutile with CCl4 for the low temperature production of TiCl4 was studied in both packed bed and fluidized bed reactors.Synthetic rutile samples before and after chlorination were characterized with SEM

XRD and XPS.Synthetic rutile produced by the Zigong process can be rapidly chlorinated by CCl4 at 450℃ to 500℃.The presence of Fe3+ ions in the lattice of the rutile phase was the key reason for the high reactivity.It was also found that an inert rutile shell was formed during the mild pre-oxidation used in the manufacturing process of the synthetic rutile material.This limited the maximum TiCl4 yield in the chlorination process to 90%.However

this inert rutile shell structure maintained the particle size during the chlorination process

it was also beneficial because it allowed the chlorination of the synthetic rutile material in a fluidized bed reactor.This process of using CCl4 for the chlorination of rutile is potentially valuable as an environmental protection technology.It effectively converts the undesirable ozone destructive substance (ODS) CCl4

an industrial byproduct

into a non-ODS product.

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