SU704654A1 - Method of processing aluminium, cobalt and molybdenum catalyst - Google Patents

Description

(54) METHOD FOR THE WORKING OF EFFICIENT ALSH -:, :: CATALYST OF THE WHOLESALE TRAILER

In it, molybdenum is mixed, the aluminum hydroxide is filtered off and subjected to gel impregnation in caustic soda solution.

The method is carried out in the following way: the spent catalyst is crushed to a particle size of 0.1 mm, mixed with soda and the resulting mixture is sintered at 850-900 s. for 1 h. Under these conditions, aluminum and molybdenum form soluble aluminate and sodium molybdate compounds; cobalt does not form soluble compounds.

The obtained sinter is leached with a mixture of caustic sodium hydroxide with a concentration of 10 A / L at a temperature of 80 ° C and a T: W ratio of 1: 7 for 1 h and the resulting pulp is filtered. The cobalt remains completely in the sediment, the extraction of aluminum in the solution is 99.5%, the molybdenum is 99.95%, the pH of the solution during leaching is 12.5-13.0.

Alkminium and molybdenum containing filtered solution is injected at a temperature of 80 ° C with carbon dioxide until the pH falls from 9.4 to 9.7. Upon reaching the specified pH, all aluminum precipitates as a hydroxide and takes part of the molybdenum with it. To completely separate molybdenum from aluminum at the end of the carbonization process, ammonium chloride is added to the pulp in an amount of 9-17% of the molybdenum content in the solution (0.18-0.2-stoichiometry) and stirred for 2 hours at a temperature of CBS After this treatment, the aluminum hydroxide is filtered from the molybdenum-containing basic solution and twice treated with caustic soda solution of a concentration of 5-10 g / l at a temperature of 20-25 ° C for 1 h to remove from molybdenum. Extraction of molybdenum from the catalyst into the solution is. 99.8 Bore waters are used in the leaching of subsequent batches of the cake, the molybdenum-containing basic solution is sent to precipitate molybdenum sulfide using sodium sulfide (consumption of Agr 6.4 g per 1 g of molybdenum in solution). After precipitation of molybdenum sulfide, the pulp is neutralized with sulfuric acid to pH 1.5-1 / 7 and boiled for 2 hours, the precipitated molybdenum sulfide is filtered off, washed with water and dried. Extraction of molybdenum in the finished product - 99.5%. Aluminum hydroxide, filtered after the second repulp in an alkali solution, contains no more than 0.1% molybdenum and corresponds to CMTU 945-4. The recovery of alcumin in hydroxide is 98.9%. .

Example 1.100 Gizelled catalyst containing 4073% Al 3, l Co and 9.36% Mo is mixed with 140 g of sodium carbonate. The mixture is placed in an alundum crucible and is sintered in an electric shaft furnace at a temperature of 870 ° C for 1 hour. The obtained sintered amount of 194.64 g is leached with a solution of caustic soda with a concentration of 10 g / l at a temperature i.e. 1: 7 for 1 hour. The pulp is filtered off, the filter cake is washed with a 10 ml / liter heated to caustic soda solution in an amount of 500 ml, and the wash water is combined with the basic solution. The total volume of solution is 1820 ml. Cobalt is not detected in the solution. The precipitate obtained is calcined at 700 ° C for 2 hours. The calcined product has the following chemical composition Co — 41.03%; L1 - 5.54%; Mo -

Carbon dioxide is introduced into a combined 1820 ml solution having a pH of 12.7. The carbonization process is carried out at a temperature of 80 ° C and continuous leaching.

After reaching RP 9.6, the supply of carbon dioxide is stopped, 0.93 is added to the pulp and stirred for 2 hours at a temperature of 80 ° C, then the precipitate is filtered off and repulsed twice at room temperature with an alkali solution of 10 for 1 hour. filtration aluminum hydroxide contains Mo - 0.09%, Fe 0.002% A1 (OH) is the rest and corresponds to CMIU 945-41, the extraction of aluminum in the hydroxide is 98.9%. Wash water sent from the leaching of the next batch of spec.

To the filtrate (V 1430 ml) containing molybdenum, 51.4 g of sodium sulphide is added at the rate of 6.5 g per

1g of molybdenum in solution. The solution is neutralized with sulfuric acid to a pH of 1.6 and maintained at boiling point for

2h The precipitated molybdenum sulfide is separated from the solution by filtration. Extraction of molybdenum in the sediment 99,5%. The aluminum content in molybdenum sulfide is 0.05%.

Example 2. The spent catalyst is processed under the conditions of Example 1. The difference is that after carbonization, 0.4 g of NH is added to the solution (4.3% of the amount of molybdenum in the solution). The precipitate of aluminum hydroxide contains molybdenum 0, 65%, 3% of aluminum has passed into the molybdenum solution. Ie.induction of aluminum in hydroxide - 95.9%, molybdenum in the finished product - 99.2%.

Claims (2)

Example 3 The spent catalyst is processed under the conditions of Example 1. The difference is that after carbonization of the solution, 1.6 g (17% of the acid molybdenum in solution) is added. Remedy hydroxide al |. Mo contains - 0.09%. Of the attraction of molybdenum to the finished product is 99.5%. Example 4. The spent catalyst is processed under the conditions of Example 1. The difference is that the pulp is mixed with ammonium chloride for 1 hour. When re-leaching with repulpation with caustic soda, a partial transition of aluminum into the solution and contamination is observed im molybdenum product Extraction of molybdenum 99.5%, aluminum - 97.5%, the aluminum content in the molybdenum product 2.5%. Example 5. The spent catalyst is processed under the conditions of Example 1. The difference is that, after the treatment of the pulp with ammonium chloride, the aluminum hydroxide is not re-leached with an alkali solution. There is an increased loss of molybdenum with an alcuminic product. The recovery of molybdenum into the final product is 90%. Aluminum hydroxide contains 2.1% molybdenum. Example b. The waste container is processed under conditions of arimer 1. The difference is that. After filtration of the hydroxide, it is repulped twice with caustic soda solution with a concentration of 20 g / l. The transition of aluminum to molybdenum-containing solution is observed, which leads to a decrease in the extraction of aluminum in hydroxide to 95% and an increase in the AI content in the molybdenum product to 0.85%. Example 7. The spent catalyst is processed under the conditions of Example 1. The difference is that the temperature during repulpable hydroxide with an alkali solution is maintained at 40 ° C. Aluminum is observed in solution. The extraction of aluminum into hydroxide is 98%, the aluminum content of molybdenum sulfide is 0.15%, Example 8. The spent catalyst is processed under the conditions of the prototype. Extraction of molybdenum to sulfide is 96%, aluminum to hydroxide is 90%. The content of alcmini in the molybdenum product is 1.2%, molybdenum in aluminum hydroxide is about 8%. The method of processing a spent alumino-cobalt-molybdenum catalyst by sintering it with soda, leaching the cake with an alkali solution and converting aluminum and molybdenum into a solution, followed by separating the solution from the cobalt-containing sludge, releasing the aluminum from the solution by carbonization with carbon dioxide, followed by the removal of the molybdenum sludge from the cobalt containing sludge. treatment of the newly obtained solution with sodium sulfide, characterized in that, in order to increase the degree of extraction of metals and villages In order to separate them, at the end of the carbonation stage, ammonium chloride is added to the pulp in an amount of 9-17% by weight of the molybeneum content, mixed, the aluminum hydroxide is filtered off and leached in caustic soda solution. Sources of information taken into account in the examination 1. The author's certificate-USSR 233919 / cl. 40a 49/00, 1967. 2. Report of the Institute of VNIIPvtortsvetmet on the topic No. 26-69-035 Method for extracting non-ferrous and rare metals from spent alkmobaltmolybdenum catalysts, Donetsk, 1971 (prototype).