SU1704036A1 - Method of checking degree of titanium tetrachloride purification - Google Patents

Abstract

The invention relates to the field of titanium metallurgy and can be used for the operational control of the process of purification of titanium tetrachloride and the assessment of its suitability in the manufacture of spongy titanium. The goal is to simplify the method, increase express speed and reduce costs. The method consists in preparing a standard — highly purified TICU with an impurity content not exceeding 0.002 mass% and recording the optical absorption spectra of the standard of the analyzed TICU under identical conditions. By the shift of the absorption edge of the analyzed TICU relative to the standard, the quality of the analyzed sample is judged. 1 tab.

Description

The invention relates to the field of titanium metallurgy and can be used for the operational control of the process of purification of titanium tetrachloride and the assessment of its suitability in the manufacture of spongy titanium.

The purpose of the invention is to simplify the method, increase express speed and reduce costs.

Example. A reference sample is prepared by the following method. Industrial production of purified titanium tetrachloride is subjected to complex purification in three stages.

The first stage is cleaning with copper powder. A portion of titanium tetrachloride and PMC grade copper powder in an amount of 1% by weight of TICU is placed in a reactor with a reflux condenser, turn on stirring, heat and incubate for 2-3 hours under these conditions.

After settling, titanium tetrachloride is decanted. In the second stage, decanted TICU are oxidized by oxygen under the influence of UV radiation. To accomplish this, titanium tetrachloride, located in a quartz tank made of optical quartz, is irradiated with UV light from a PRK-4 lamp with continuous bubbling of oxygen gas through the TICU. The exposure time is at least 6 hours at ambient temperature.

The third stage - final purification by rectification. After photo-oxidized, titanium tetrachloride is poured into a cube of a laboratory distillation column made of glass, the rectifying part of which (0.6 m high) is filled with a Levin nozzle, the rectification mode is periodic, the number of separation steps is three (determined experimentally from the model mixture

one

W

about

TiCU -). The column operates in the neutral mode for 3 hours to reach equilibrium, after which fractional sampling is started at a rate of 0.02 l / h. The first fraction containing the lower-boiling impurities (.. 136.6 ° C at P 1 atm), and the third (vat residue) containing the above-boiling impurities (g. 136.6 ° C at P 1 atm), taken in the amount 20% by weight of the original discarded. The average (second) fraction "; booth. 136.6 ° C at P 1 atm), which is a colorless liquid, is a reference and has the following composition, in wt.%: Cobalt. 0.0001 - 0.0002; 8.0 × 0.0001 - 0.0002; Fe 00002; AI 0.0001: S 0.0002; Y - 0.0001; Cr 0.0002; Mp 0.0001; Sn 0.0002; Si 0.0001; Ir 0.0003; NI 0.0001; Mo 0.0002.

The content of the determined impurities in the obtained standards is at the limit of sensitivity of the existing methods.

The standard preparation method used gives reproducible results. If all the purification parameters and analysis methods are observed, regardless of the composition of the original industrial purified TiCU, the impurity content in all reference samples corresponds to the above composition, and the edge of the absorption band (if the measurement conditions are strictly observed) is characterized by a frequency of 26,850 ± 5.

To check the depth of purification of the standard. :: i nl, it was subjected to additional purification; for this purpose, the reference sample of titanium tetrachloride obtained by the method written off above, psperperly oxidative purification in molten sodium chloride. tetrachloride T T –U-E using a rasa carrier (purified and dried argon) was fed to the reactor with a molten mixture of chloride i, s: reel and sodium nitrate, having a temperature of 900 ° C. the amount of NaNOa 2% by weight of NaCl. After bubbling through the melt, TICM pairs were condensed and collected in a receiver. Analysis of the treated standard according to the existing methods of display ;; coincidence with the composition of the initial standard. In parallel, the electron absorption of an additionally purified standard was removed. The absorption band edges were characterized by a frequency of 26852.

The resulting high purity TICU was placed in a cuvette under conditions that excluded

the effect of atmospheric gases and moisture was sealed and used in the future. as a reference (constant). The cuvette is a sealed tube with a diameter of 15 mm with a domed taps.

Sample preparation.

Titanium tetrachloride from the industrial pipeline is taken directly in the duct into the cells described above under conditions which exclude the influence of atmospheric

gases and moisture.

Perform control. The prepared cuvettes with the zhalon and the test sample are placed in the cuvette compartment of the Specord-UUSiS spectrophotometer and the electronic absorption spectra are taken. In order to obtain reliable results, the position of the edge of the TICU absorption band is taken at half the optical density of the instrument, since the boundary

. bandwidths in the spectrum are subject to distortion. The shift of the edge of the absorption band of each sample relative to the reference is measured. The results are presented in the table.

All measurements should be carried out under identical conditions, since reproducible results can only be achieved if the measurement conditions are strictly observed (layer thickness, measurement geometry, cuvette material, and conditions for taking a sample into the cuvette).

The TICU analyzed is classified as first grade with a shift of 600-1850 cm. to the side of the variety - with a shift of 2000 - 3430.

Claims (1)

Invention Formula The method of controlling the degree of purification TICU. including the growth of the studied TiCU with the reference, about tl and.chv.yu and with the fact that, in order to simplify and increase the speed of the process and reduce costs, a TICU standard with a total impurity content of not more than 0.002% by weight is fixed The electronic absorption spectra of the TICU and the reference measure the shift of the edge of the TiCU absorption band relative to the reference and, by the shift, judge the degree of purification of the TiCU. The position of the absorption band edge, cm (frequency) The amount of shift, cm 598,852. 1850. 1100. 1350. 12G7 1997, 2250. 2349, 3030. 3430. 3229 7093. 8098, 5096, 6254. 86 80. 4757  Product quality High-purity TICU (standard) Purified TICU, I grade Purified TlCk II grade Technical TlCk