A method of processing titanium slag

 

(57) Abstract:

The invention relates to the metallurgy of titanium and can be used in the processing of such raw materials chlorine method. The technical result is the possibility of stable operation when changing performance charator and reduce losses titanium tetrachloride with the exhaust gases. The method comprises mixing a source of slag with a reducing agent and chlorine in molten alkali metal chlorides with obtaining the calibration gas containing titanium tetrachloride, salt cleaning ASG in molten chlorides, the return of the melt after salt treatment in charator, condensation of chloride impurities in irrigation scrubber circulation resulting pulp in circuit charator in the amount of 2.0 to 3.0 t/t TiCl4and in the contour irrigation scrubber in the amount of 80-100 t/t TiCl4, condensation of titanium tetrachloride in irrigation capacitors with consistent use as irrigation liquid TiCl4with a temperature of 90-105oWITH, 25-40oC, 0-(-15)oC. the Chlorination slag in the melt is carried out at a temperature not exceeding 750oWhen the concentration of TiO21-4 wt.%, reductant - 3-5 wt.%, when the ratio is in is carried out at a molar ratio of alkali metal chloride to the amount of impurity chlorides of iron and aluminum more than 1 in the slag and CBC, respectively. 4 C.p. f-crystals.

The invention relates to the metallurgy of titanium and can be used in the processing of such raw materials chlorine method.

The main industrial method of processing titanium raw material is chlorination in the salt melt titanium slag.

There is a method of processing titanium slag with obtaining titanium tetrachloride, including the preparation of batch grinding of slag and the reducing agent, such as coke, mixing these components, the loading XLERATOR a mirror of molten chlorides of alkali and alkaline earth metals and chlorination with gaseous chlorine or anode chlorine gas at a temperature of 750-800oC and continuous renewal of the melt. In formed during the gas-vapor mixture is transferred titanium as titanium tetrachloride and chlorides of the impurities. Gas-vapor mixture is cleaned from impurities in the condensing system using hollow capacitors to remove dust; salt purification from chloride impurities, mainly aluminum, iron, condensation of chloride impurities is carried out in irrigation scrubber and condensation of titanium tetrachloride in irrigation capacitors.

The chlorination process is carried out with the conclusion Naroch Rasul titanium tetrachloride, consistently clear of solid chlorides. Cleaning is performed first from the more high-boiling liquid and solid chlorides, and then separating the solid chloride from gaseous salt purification and condensation of chloride in irrigation scrubber and irrigation capacitors for final dolabellane titanium tetrachloride. The pulp titanium tetrachloride obtained after irrigation scrubber serves for irrigation in the circuit of irrigation scrubber circuit charator - chlorination process (see "Titan", Ed. by C. M. Abundant, M.: metallurgy, 1983, S. 273-300).

The method has disadvantages, which are as follows.

Remove dust from solid chlorides in hollow capacitors leads to the formation of commorating Smoking sublimates, which makes their further processing.

The circulation of the pulp from irrigation scrubber in charator provides heat removal, but you can't adjust it depending on the performance of charator. The same thing happens when the circulation of the pulp in the irrigation system scrubber. The circulation of the pulp does not provide the required heat removal and washing of the gas-vapor mixture of titanium tetrachloride from impurities chloride gelee and technical-economic indicators of the process.

The technical result of the claimed invention is the possibility of stable operation regardless of changes in performance charator and enhance the yield of titanium tetrachloride by reducing its losses with the exhaust gases.

The technical result is achieved in that in the method of processing titanium slag with obtaining titanium tetrachloride, including the preparation of a charge, load it in charator, chlorination with chlorine or anode chlorine gas in the melt of metal chlorides with continuous update of the melt with getting gas mixture containing titanium tetrachloride, salt cleaning gas mixture, the condensation of chloride in irrigation scrubber circulation resulting slurry loop irrigation scrubber circuit charator for filing in the process of chlorination and subsequent condensation with the Department of titanium tetrachloride in irrigation capacitors according to the invention a salt treatment in molten chlorides lead directly after chlorination, the salt chlorination and cleaning is performed at a molar ratio of alkali metal chloride to the amount of impurity chlorides of iron and aluminum more than 1.0 in the slag and in Paraguay pulp in circuit chlarotera, supplied to the cooling when the chlorination is 2,0 - 3,0 t/t titanium tetrachloride, and the contour irrigation scrubber - 80-100 t/t titanium tetrachloride;

in addition, condensation of titanium tetrachloride in irrigation capacitors carried out successively using as irrigation liquid titanium tetrachloride with a temperature of 90-105oC, titanium tetrachloride to a temperature of 25-40oC and titanium tetrachloride with temperature 0-(-15)oC, respectively;

the chlorination is carried out at a temperature not exceeding 750oC at a concentration of titanium dioxide and a reducing agent in the melt 1-4 and 3-5%, respectively, when the ratio of chlorine to slag of 1.48-1.62 and maintaining the linear velocity of the feed glorieuses agent within 30-20 m/sec in each tuyere.

The method consists in the following.

The conducting salt purification immediately after chlorination allows you to more effectively capture the admixture of solid chlorides of iron and aluminum, as well as particles pylones (crushed fraction of the charge). The melt after salt purification return to chlorination, which allows more rationally reagents are alkali metals and effective espresso material improves the extraction of titanium from the feedstock. Chlorination of raw materials and salt cleaning gas mixture after chlorination should be carried out at a molar ratio of alkali metal chloride to the amount of impurity chlorides of iron and aluminum more than 1.0 in the slag and in the vapor-gas mixture, respectively. It is the ratio of the components in the chlorination reduces the removal of these impurities in the gas-vapor mixture, and salt cleaning effectively removes these impurities from the gas mixture. At the next stage gas-vapor mixture is cleaned in irrigation scrubber; for irrigation use pulp titanium tetrachloride. The slurry of the titanium tetrachloride from the scrubber at a ratio of 2.0 to 3.0 t/t titanium tetrachloride return in charator for sterilization temperature chlorination. The last stage of cleaning gas mixture titanium tetrachloride in irrigation capacitors hold speed using as irrigation liquid titanium tetrachloride with a temperature of 90-105oC, 25-40oC and with a temperature of 0-(-15)oC. Modes of circulation of the pulp in the contours of charator and irrigation scrubber not only effectively perform the heat removal and cleaning from impurities, but also depend on the performance of chlarotera, the sama is - etyrechmernogo titanium. When changing performance charator change the ratio of the number of circulating pulp in circuit charator and scrubber at stated intervals and ensure the stability of the whole technological cycle.

On the effectiveness of the chlorination process is influenced by other declared parameters. The concentration of titanium dioxide and a reducing agent in the melt during chlorination 1-4 and 3-5 wt.%, accordingly, the temperature of the chlorination of not higher than 750oC prevent boiling of the melt during the chlorination, and the ratio of chlorine and slag (1,48-1,62):1 and the linear velocity of the gaseous feed glorieuses agent allow you to provide the most effective crushing in the thickness of the melt, uniform distribution and at the same time reduces the destruction of the tuyere site, prolonging its service life.

Modes of condensation of titanium tetrachloride in irrigation capacitors, a sequential decrease of temperature of the irrigating fluid lead to the most complete capture and condensation of titanium tetrachloride, thereby reducing the possibility of loss of titanium tetrachloride with process gases.

Substantiation of the parameters.

When mo is camping out impurities in the gas-vapor mixture. When the molar ratio of alkali metals and chlorides of the impurities of aluminum and iron is less than 1.0 when the salt reduced cleaning efficiency of cleaning from dust and solid chlorides of aluminum and iron.

The number of circulating pulp in circuit charator less than 2.0 t/t titanium tetrachloride does not provide the necessary heat removal, and increases the temperature of charator. The increase in the number of circulating pulp in circuit charator more than 3.0 t/t titanium tetrachloride leads to a decrease in melt temperature of chlarotera, reducing the rate of chlorination. In addition, there is condensation of solid chlorides on the set of charator. The number of circulating pulp titanium tetrachloride in the circuit of irrigation scrubber is less than 80 t/t titanium tetrachloride leads to poor heat removal and, consequently, reduces the effectiveness of titanium tetrachloride purification from impurities. The number of circulating pulp titanium tetrachloride in the circuit of irrigation scrubber more than 100 ton/tons titanium tetrachloride reduces the efficiency of cooling the circulating slurry and increases energy consumption.

The temperature of 90-105oC irrigation liquid titanium tetrachloride at perched deposition of impurities on the surface of the heat transfer equipment. When the temperature of the irrigation fluid above 105oC decreases the degree of condensation of titanium tetrachloride on the first level. The temperature of 25-40oC irrigation fluid at the second stage condensation irrigation ensures optimum energy consumption at the stage of condensation. At temperatures below the 25oC increase the energy consumption for cooling the circulating fluid. At temperatures above 40oC decreases the degree of condensation of titanium tetrachloride in the second stage. Temperature 0-(-15)oC irrigation fluid provides the optimal combination of effective trapping titanium tetrachloride and energy consumption. At temperatures above 0oC decreases the degree of catching titanium tetrachloride and the losses increase with the exhaust process gas. At temperatures below -15oC dramatically increase energy costs, which practically does not increase the degree of trapping titanium tetrachloride.

The method is illustrated by an example.

Chlorination is subjected to titanium slag containing TiO285-88 wt.%. Titanium slag is crushed and mixed with coke to obtain a mixture. The chlorination is carried out at a temperature of 700oC in the melt soleus%. when the molar ratio of chloride of potassium and sodium to the sum of the chlorides of iron and aluminum is more than 1.0. In charator serves anode chlorine gas on the 4th chloropetalum with the linear feed speed of 20-30 m/sec. when the ratio of chlorine and slag (1,48-1,62):1. The resulting vaporous chlorides in the form of vapor mixture (CBC), containing titanium tetrachloride and the chlorides of iron, aluminum, potassium and sodium, with a temperature of 300-500oC is coming to salt treatment in salt scrubber. Salt treatment in molten alkali metal chlorides at a molar ratio of alkali metal chlorides to the amount of chloride impurities of 1: 1.5 of the calibration gas in the melt is transferred unreacted particles of the mixture, the solid chlorides of iron and aluminum. After saturation of the melt his return in charator. Partially purified salt scrubber ASG comes in irrigation scrubber, where it is further cleaned ASG from the chlorides of iron, aluminum and other high-boiling chlorides (Na, K). As irrigation fluids used pulp titanium tetrachloride obtained in the condensation process. In irrigation scrubber is the capture of solid chlorides of the impurities and partial condensation of the titanium tetrachloride with the formation of the pulp, which is napravliati 80-100 t/t titanium tetrachloride - in the path of the irrigation scrubber for cooling of the pulp. Purified ASG is directed to step condensation in irrigation capacitors. The first stage of the condensation is carried out at a temperature of 90-105oC, and the second 25-40oC and the final condensation of titanium tetrachloride is carried out at 0-(-15)oC. the Final product is a liquid titanium tetrachloride is removed from the irrigation system condensers.

The output of titanium in the final product is 96%.

1. A method of processing titanium slag with obtaining titanium tetrachloride, including the preparation of a charge, load it in charator, chlorination with chlorine or anode chlorine gas into the molten metal chlorides with continuous update of the melt with getting gas mixture containing titanium tetrachloride, salt cleaning gas mixture, the condensation of chloride in irrigation scrubber circulation resulting slurry loop irrigation scrubber circuit charator for filing in the process of chlorination and subsequent condensation with the Department of titanium tetrachloride in irrigation capacitors, characterized in that that salt treatment in molten chlorides lead directly after hariramani the th chlorides of iron and aluminum more than 1 in the slag and in the vapor-gas mixture, respectively, the melt after purification sent to the chlorination process, the number of circulating pulp in circuit charator supplied to the cooling when the chlorination is 2,0 - 3,0 t/t titanium tetrachloride, and the contour irrigation scrubber - 80 - 100 t/t titanium tetrachloride.

2. The method according to p. 1, characterized in that the condensation of titanium tetrachloride in irrigation capacitors carried out successively using as irrigation liquid titanium tetrachloride to a temperature of 90 - 105oC, titanium tetrachloride to a temperature of 25 - 40oC and titanium tetrachloride with temperature 0 - (-15)oC.

3. The method according to p. 1, wherein the chlorination is conducted at a temperature not exceeding 750oC at a concentration of titanium dioxide and a reducing agent in the melt 1 - 4 and 3 - 5%, respectively.

4. The method according to p. 1, wherein the chlorination is carried out at a ratio of chlorine to slag (1,48 - 1,62) : 1.

5. The method according to p. 1, characterized in that the linear feed speed glorieuses agent is maintained within the range of 20 - 30 m/s

 

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