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Simultaneous Recovery of Nickel and Aluminium From Spent Reformer Catalyst
Simultaneous Recovery of Nickel and Aluminium From Spent Reformer Catalyst
residue treated with HNO3 (1:1) at 60C to dissolve nickel in the solution. Vicol et al. (1986)
studied leaching of spent catalyst with an aqueous solution of 15-23% ammonia at 60-90C
at pH 7.5-9 and nickel was recovered as nickel nitrate. Sinka et al. (1988) studied extraction
of nickel from spent nickel catalyst based alumina (NiO/Al 2O3) leaching with sulfuric acid
solution 90% nickel was recovered. Ganguli et al. (1988) studied spent nickel catalyst with
32% hydrochloric acid concentration at 70C and nickel recovery was found to be 96%.
Molnar et al. (1988) reported a spent hydrocracking catalyst roasted at 390C with NH 4Cl,
leaching with water at 80C and crystallization as NiCl 2 at 85% nickel yield. Pamela et al.
(1991) studied reduction roasting-sulfuric acid leaching of nickel from spent nickel catalyst.
About 98% of nickel was recovered as nickel oxide under the following conditions: sulfuric
acid concentration: 1.87 M; reaction time: 2 h.; reaction temperature 80C. Chaudhary et al.
(1993) studied leaching the low-grade spent catalyst with hydrochloric acid. They obtained
low Ni extraction efficiency (only 18%). Sibban Singh (1993) studied leaching spent nickel
catalyst with 1-3 normal nitric acid at 100C for 1-3 h. Khanna et al. (2000) studied
reclamation of nickel catalyst from spent catalyst by dry reduction method. The study
investigates the leaching aluminium and nickel from spent catalyst (NiO/Al 2O3) with caustic
soda and aqua regia. The process conditions studied include caustic soda and aqua regia
concentrations, temperature, time and solid-liquid ratio.
Experiment
Materials and Apparatus
The spent reformer catalyst used in this study was provided by RCF (India). The grayish
black rings of spent catalyst were crushed and powdered. The reagents like Na 2CO3, H2O2,
H2SO4, HCl, HNO3, NaOH, used were of AR grade. The reaction between spent catalyst and
caustic soda and aqua- regia was performed in a 500-mL round bottom flask on hot plate.
Procedure
Hundred gram of spent catalyst was added at a time to the agitated caustic soda solution
(200-mL) of the required concentration, time and temperature. The leached solution was
filtered. Aluminium was dissolved into sodium aluminate and pH was adjusted to 5-5.5 by
adding dilute sulfuric acid Aluminium precipitated as aluminium hydroxide was converted into
its oxide. The residue left after removal of aluminium is then digested with aqua-regia at
100C for 2 hrs and filtered. To the filtrate containing Ni, Fe, Al, and Mg was added H 2O2 and
Na2CO3 and pH was adjusted to 5-5.5 Al/Fe precipitates its hydroxide and its removed by
filtration. Then the pH was adjusted at 6.5 by adding NaF/HF to precipitates Mg as MgF 2 to
obtained nickel sulfate solution and its precipitate which was convert carbonate by adding
Na2CO3. The amount of sulfuric acid was added to it and recovery of nickel in the form of
nickel sulfate crystals was found to be 95-96%. The samples were analyzed for determination
of metals content using spectrophotomery and atomic absorption spectroscopy (AAS). After
that the percentage of nickel and aluminium were calculated.
Results and Discussion
Effect of caustic soda concentration on extraction of aluminium
The effect of caustic soda concentration on leaching of spent nickel catalyst was studied
using different concentrations in the range 5-25% at a constant temperature at 80C. The
solid/ liquid ratio was kept constant at 1:2 g/mL. The results are shown in (Fig.1). The caustic
soda concentration also has a pronounced effect on the dissolution of Al 2O3. About 97.4% of
the Al present in the spent catalyst were extracted using 20% caustic soda solution after 120
min.
significant effect on dissolution of nickel aluminium oxide. After 2h leaching time 97.7% Al,
and 98% Ni were extracted.
Recovery
(%)
1/1
96.60
1/2
97.40
1/2.5
97.40
1/3
97.40
While in case of nickel the S/L ratio 1/3 g/ml. was found to be best for nickel extraction and
the S/L ratio increases upto 1/4 g/ml.the extraction efficiency negligible. The results are
shown in Table 2.
Table 2. The effect of Solid/ Liquid ratio on leaching
efficiency and the concentration of Nickel in the aquaregia
S/L ratio {g/ml)
Recovery (%)
1/1
40.0
60.0
1/2.5
97.70
1/3
98.0
98.0
Conclusion
1. The spent catalyst needs to leached with NaOH at 90-100C to form soluble
aluminium compound and it is easy to recovery of aluminium.
2. The rate of extraction of aluminium was found maximum at temperature 80C further
increase temperature no adverse effect on aluminium extraction.
3. Very high recovery of aluminium obtained in very short time.
4. The residue left after recovery of aluminium leaching with aqua regia at a
temperature 90-100C dissolution 2 hrs. Could bring 98% of nickel in solution.
5. Recovery of nickel as NiSO4.7H2O crystals was obtained 95-96%.
Reference
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