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Method for recycling molybdenum from waste hydrogenation catalysts

A waste hydrogenation catalyst, ammonium molybdate technology, applied in chemical instruments and methods, molybdenum compounds, inorganic chemistry, etc., can solve the problems of low recovery efficiency, less research, and large salt consumption in chemical precipitation

Active Publication Date: 2021-05-18
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the recovery efficiency of the chemical precipitation method is low, and the process is not suitable for control; the ion exchange method has the disadvantages of a long cycle and a large amount of salt consumption.
The recovery of metals by solvent extraction is not only efficient but also simple. At present, the commonly used organic solvents for extracting molybdenum mainly include acidic extractants, neutral extractants and amine extractants, while there are few studies on the recovery of molybdenum by chelating extractants.

Method used

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  • Method for recycling molybdenum from waste hydrogenation catalysts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Grind 50 g of spent hydrogenation catalyst and 100 g of red mud evenly, and roast them at 300°C for 1.5 h; after the calcination is cooled, leaching with water at 70°C for 40 min at a leaching liquid-solid ratio of 5:1, Molybdenum leaching rate was 95.72%.

[0027] (2) Use 30 wt.% sulfuric acid to adjust the pH of the leaching solution in step (1) to 6~8, and precipitate aluminum hydroxide; extract the remaining liquid, and extract the organic phase component into Kelex 100 (10 wt.%)+ Sulfonated kerosene (90 wt.%), Acoega M5640 (10 wt.%) + sulfonated kerosene (90 wt.%), Acorga M5774 (10 wt.%) + sulfonated kerosene (90 wt.%), AcorgaOPT5540 ( 10 wt.%)+sulfonated kerosene (90 wt.%), the O / A ratio of the extracted organic phase to the aqueous phase is 1:1, the extraction time is 5min, the extraction temperature is 25°C, and the extraction of molybdenum after the primary extraction The rates were 64.52%, 86.21%, 87.12%, and 87.85%, respectively.

[0028] (3) Back-extra...

Embodiment 2

[0030] (1) Grind 50 g of spent hydrogenation catalyst and 100 g of red mud evenly, and roast at 300 °C for 1 h; after the calcination is cooled, the leaching liquid-solid ratio is 5:1, and leaching with water at 70 °C for 60 min, the molybdenum leaching rate was 95.73%.

[0031] (2) Use 30 wt.% sulfuric acid to adjust the pH of the leaching solution in step (1) to 6~8, and precipitate aluminum hydroxide; extract the remaining liquid, and extract the organic phase component into Mextral 84-1 (20 wt.% ) + sulfonated kerosene (80 wt.%), Mextral860N-1 (20 wt.%) + sulfonated kerosene (80 wt.%), Mextral 973N (20 wt.%) + sulfonated kerosene (80 wt.%) , Mextral 984N (20 wt.%) + sulfonated kerosene (80 wt.%), extract the organic phase compared with the aqueous phase O / A is 1:1, the extraction time is 5 min, the extraction temperature is 25 ° C, after the primary extraction The extraction rates of molybdenum were 12.11%, 15.54%, 15.78%, and 16.12%.

[0032] (3) Back-extract the organi...

Embodiment 3

[0034] (1) Grind 50 g of spent hydrogenation catalyst and 80 g of red mud evenly, and roast at 500°C for 1 h; after the calcination is cooled, the leaching liquid-solid ratio is 4:1, and leaching with water at 60°C for 40 min, the molybdenum leaching rate was 96.12%.

[0035](2) Use 30 wt.% sulfuric acid to adjust the pH of the leaching solution in step (1) to 6~8, and precipitate aluminum hydroxide; extract the remaining liquid, and extract the organic phase component into Kelex 100 (30 wt.%)+ Sulfonated kerosene (70 wt.%), Acorga M5640 (30 wt.%) + sulfonated kerosene (70 wt.%), Acorga M5774 (30 wt.%) + sulfonated kerosene (70 wt.%), AcorgaOPT5540 ( 30 wt.%)+sulfonated kerosene (70 wt.%), the O / A ratio of the extracted organic phase to the aqueous phase is 1:1, the extraction time is 5min, the extraction temperature is 25°C, and the extraction rate of molybdenum after primary extraction 81.11%, 96.24%, 96.18%, 96.32%.

[0036] (3) Back-extract the organic phase extracted in...

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Abstract

The invention discloses a method for recycling molybdenum from waste hydrogenation catalysts and belongs to the technical field of recycling of solid wastes. The method comprises the following steps: mixing the waste hydrogenation catalysts with red mud according to a ratio, crushing and grinding uniformly, and roasting and leaching in water; adding acid into a leaching solution to adjust the pH value, and selectively extracting molybdenum from a molybdenum-containing acid solution after aluminum hydroxide is separated out through a chelating extraction agent; carrying out back extraction on the molybdenum-containing organic phase by using ammonia water, ammonium salt or a mixed solution of the ammonia water and the ammonium salt; and adding an impurity removing agent into a back extraction solution to remove impurities such as P and Si, adjusting the pH value by using hydrochloric acid, and concentrating, evaporating and crystallizing to obtain an ammonium molybdate product. According to the method, the problems that the traditional sodium salt roasting energy consumption is high and the corrosion property is strong are solved; efficient extraction of metal molybdenum is achieved through the chelating extraction agent; the impurities are removed before preparing ammonium molybdate; the comprehensive recovery rate of molybdenum is greater than 85%; and the method has a certain application value.

Description

technical field [0001] The invention belongs to the technical field of solid waste recovery and utilization, and relates to a method for recovering molybdenum from waste hydrogenation catalysts. Background technique [0002] Hydrogenation catalyst is one of the most commonly used catalysts in petroleum refining process, mainly composed of carrier alumina and active components molybdenum, nickel, silicon and so on. Hydrogenation catalysts will lose their activity under the influence of high temperature working conditions and metal deposition during use, so a large amount of spent hydrogenation catalysts are produced every year. Spent hydrogenation catalyst is an important secondary resource containing valuable metals such as nickel, chromium, vanadium, molybdenum, and aluminum. The recycling of spent catalysts can not only reduce the pollution to the environment, but also recover valuable metals to prepare catalysts again, which has certain economic benefits. [0003] For...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/34C22B7/00C22B1/02C22B3/40C01G39/00
CPCC22B34/345C22B7/006C22B1/02C01G39/00Y02P10/20
Inventor 曾曼彭明国毛林强桂松王嘉张文艺
Owner CHANGZHOU UNIV
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