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Journal of the Korean Chemical Society (JKCS)

ISSN 1017-2548(Print)
ISSN 2234-8530(Online)
Volume 4, Number 1
February 20, 1957 

Preparation of Titanyl Chlorde

염화티타닐 제조에 관한 연구
Yoon Kyung Shin, Byong Doo Chyun

신윤경, 천병두
1. Preparation of Titanium tetrachloride; The following precesses were strictly followed as the preliminary step to obtain pure TiOCl2, titanyl chloride; First, pure Titanium Oxide mixed with carbon is rolled into pills. After drying up perfectly, these pills are heated at 900∼1000℃. And then the pills are subjected to the flow of Cl2 gas in a quartz tube heated to 900-1000℃. Thus Titanium tetrachloride is obtained. 2. Preparation of TiOCl2 ; Yellowish trobrown solution is made by pouring 80 g of conc. HCl ( 1.19) to 45 gr of Titanium tetrachloride (approx. 2 times of theoretical amount). Then this solution is kept settled for 5-days in a desiccator filled with phosphorous pentoxide at room temperature. As the colorless amorphous solid thus obtained is washed with aceton, 36.5 g of the pure salt are obtained. 3. Determination of composition. The analysis of the sample taken from the deposit desiccated gives the following data; (A) Qualitative analysis; a) Ti(OH)4 is precipitated by adding NaOH in water solution of the salt. b) Adding AgNO3 solution, the water solution of the salt gives white precipitate of AgCl. c) When acid and H2O2 are added, the solution turns its color to redish brown (This proves that TiO++ was converted into TiO2++ by oxidation of H2O2. (B) Quantitative analysis; a) Ti(OH)4 precipitated by 10% NaOH isalitatsubjected consecutively to the filtration and ignition in porcelain crucible at approx. 1000℃, then TiO2 thus formed is weighed and calculated into Ti content. b) Chlorine involved in water solution of the salt is determined by Vorhardt method. Result: The values obtained from previous analysis, devied by their atomic weight gives the following composition: Ti : Cl = 1 : 2 Therefore TiOCl2 should be given as its molecular formula. 4. Summary. When TiCl4 is additated into conc. HCl, TiO++ formed exists as a stable form, and forms TiOCl2. However TiOCl2 is unstable to heating. When the temperature is raised to 65℃, the decomposition of the solution is accelerated, and gives TiO2 aq. TiOCl2 in addition is highly hygroscopic.
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