SU1452144A1 - Method of processing spent melt of titanium chlorates - Google Patents

Abstract

The invention relates to methods for processing waste melts of titanium chlorinators. The purpose of the invention is to increase the selectivity of scandium extraction and increase its concentration in the target product. The waste water is leached and the insoluble residue is separated from the solution by filtration. The resulting solution is treated with alkaline reagents to precipitate hydroxides of non-ferrous and rare metals. The precipitate is treated with an alkaline solution of hypochlorite, filtered and get a rough rare metal concentrate. The latter is dried, calcined, and chlorinated in the molten alkali and / or alkaline earth metal chlorides at 700-900 ° C. In this case, the main part of ferric, titanium and zirconium chlorides sublimates. The melt containing scandium, thorium and a number of impurities is dissolved, the solution is sent for sorption extraction of scandium. After elution, rare metal concentrate containing scandium, thorium, iron, chromium and other impurities is precipitated from the eluate. In the process, an increase in the selectivity of scandium extraction due to its purification at the chlorination stage of titanium (100%), zirconium (60-99%) is achieved , chromium (by 30-40%) and iron (by 40-90%), as well as an increase in the concentration of scandium oxide in the target product to 53% (3.3 times). 1 tab.

Description

The invention relates to non-ferrous metallurgy and can be used in the complex processing and decontamination of chloride wastes generated during the chlorination of ilmenite concentrates, in particular for the processing of waste titanium chlorinators with the extraction of valuable components and the production of various commercial products; compounds of scandium, thorium, titanium, br} rki, obtaining iron oxide pigments, inorganic sorbents of hydroxy-hydrate type, chromium pigments, etc.

The purpose of the invention is to increase the selectiveness of scandium extraction and increase its concentration in the target product.

3U52t44

Example 1, Spent compacted elute was precipitated with x-metal chlorate precipitate concentrate. After washing, drying

In the case of microorganism of water at W: T 2 in those and calcining at a concentrate of 2 hours at peremegaivani. Perast- held, May, Z: 53 SejOj, 43 ThO,,

0.29 TlO, 0.33 /.rOt 1 Fe-; 0j, 2.2.

BopnMijft the residue is filtered. The filtrate and insoluble residue promoters were combined. The resulting solution had the following composition, g / l: 0.03 Se} 0.05 Th; 0.3 Ti; 0.08 Zr; 28 Fe; 1.5 Cr. Deposition of color.

0.29 TlO, 0.33 /.rOt 1 Fe-; 0j, 2.2.

The rationale for the selected temperature regime of the chlorination process 10 is given in Example 2.

Example 2. ChRMK was obtained

rare and radioactive metals are pro-according to the procedure described in the example of 2 n. a solution of hydroxide nepre 1, and contained, by weight, 5Eg 0.35 So, ri (pH A, 3-4.5), previously Thi, 7.2 Ti, 0.3 Zt, 18.3 Fe three-fold iron up to two-, 16, and 2.4 Cr. with iron scrap at 90 ° C, |

For better filterability of the precipitate in tiynT.iiy 0.2% 0.2% - Hbtrt solution poly-P1 | silt || d-h (11LL), V

 DD, iV ,,,, - JSIO.

ChRMK chlorination experiments were carried out analogously to example 1 according to the npc / yia method, but the second

After fshi.troppni and washing the precipitate 20 Interpol 600-1000 C. As an alkaline solution of the hydrochlorinating agent was used,

sodium rochlorite (70 g / l NaOCL, gaseous chlorine and chlorine air

50 g / l NaOH) at 7 ° C for 2 h. Mixture (70% C). The results of the experiments

The precipitate was separated from the solution, washed with 0.25% sodium hydroxide solution and water. The dried sludge, mssdstavl ka oy a draft rare g, -shlny concentrate (PKMK), had the following composition%: 0.26 Se; 0.48 Th; 7.8 TiO; 0.3 Zr; .18.3 Fe; 3.5 Ct.

100 g of ChRMK were calcined for about 2 hours and loaded together with 200 g of spent electrolyte of magnet electrolyzers and 40 g of charcoal into a salt chlorinator. The content i melted at. 900 s and carried out the supply of chlorine through the melt layer at a rate of 2 l / min. Sublime. chlorides were trapped in the system of Kodenderder, May, Z: 53 SejOj, 43 ThO,,

0.29 TlO, 0.33 /.rOt 1 Fe-; 0j, 2.2.

The rationale for the selected temperature regime of the chlorination process is given in Example 2.

Example 2. ChRMK was obtained

presented in the table.

26 The data obtained show that at the temperature of svepie there are significant losses of scandium with the vapor-gas mixture (up to 11.5Z at). At a temperature, the chlorination process is almost impossible to conduct, due to the high melt viscosity. The use of chlorine-air mixture somewhat reduces the selectivity of the process.

Thus, chlorination of the FBM is advisable to be carried out at 700-900 chlorine or chlorine air mixture, which will ensure the maximum degree of scandium extraction and the highest

35

c.iitHn, The process was conducted for 80 min. 0 selectivity of the process.

To stop the increase in the mass of metal chlorides in the condensation chamber. By the end of chlorination, the melt rspstormli in water at W: T 2.5-3. After separation of the unreacted coal and the insoluble residue, a hardening agent was obtained, containing, g / l 0.52 Se; 0.76 Th; 0.007 Ti; 0.01 Zr; 4.7 Fe; 3.1 Cr. 500 ml of such rast45

Example 3. Same as in Example 2, except that an equimolar mixture of sodium and magnesium chlorides was used as the melt.

The chlorination process of the rare metal concentrate was carried out at 800 ° C. The results of the analysis of the initial melt, chlorinated melt and sublimates showed that the loss of scandum pore preliminarily reduced gQ with sublimated chlorides made up 2.4% of the total ferrous iron, and the separation factor of the scrottles with 30 g cation exchanger KFP-12.din and Tories from titanium and zirconium 310.

G, orP (X11yu whether at 80t7. ° C, speed The way to ensure “flight no.

". Ilstroylniya rlstpor chsrop-sorbylbirthliness layer with sclidine tciirn 1 Y1 / MI see. At the end of the program, gg el account of its purification at the stage of chlorination ion was removed by 1 n dissolution from titanium (100%), with sulfur. hydrochloric acid, water and deposits (60–99%), chromium (39–40%) metal desorption of 500 ml 3 iron (by 40–90%), as well as an increase in sodium carbonate solution. scandium oxide

Example 3. Same as in prier 2, only an equimolar mixture of sodium and magnesium chlorides was used as the melt.

The process of rare-metal concentrate was carried out at 800 ° C. The results of the analysis of the initial melt, chlorinated melt and sublimates showed that the loss of scandium with sublimated chlorides was 2.4%, and the coefficient of separation of scannable needles for prolacto from 16.5 to 53Z, t. e. n 3.3 times

Claims (1)

Invention Formula The method of processing waste plutyup titanium chlorinators, including their leaching, implantation of impurities from plants, ointment, hydrochloride, hydrochloride, hydrochloride, hydrochloride, hydrochloric acid, glop, treatment, treatment, treatment, treatment, treatment, treatment, treatment, etc. P) pof rvn "d | 1" t "l11 (1st imimtwT rt,)" lorator of the quarter t} 0g, BUT g, hijack 20. g. Smroet "lor mln" uio oi "R r" iieil ems l / mn , p "t" lorum n 1h. "00IMCOCM Madoog R epl - 1452144 rare metal concentrate and after it (C1 is extracted from it by scandium sorbts and precipitating, which is due to the fact that, in order to increase the selectivity of scandium extraction and increase its concentration in the target product, before removing scandi, the rough red-metal f - Concentrate of treatment of gas with chlorine or chloropropane mixture of chlorides of alkali and / or alkaline earth metals prn TOO-ROO C. {arvotrvit ter layer m «I1M vrip etNiMira