Method of recovering molybdenum and cobalt from waste cobalt-molybdenum catalyst

A catalyst and catalyst quality technology, applied in the field of recovering precious metals, can solve the problems of unsuitable popularization and application, high labor intensity, incomplete separation, etc., and achieve the effects of favorable cost control, improved recovery rate and low price

Active Publication Date: 2013-05-01
JINGMEN GEM NEW MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Existing methods for recovering metal cobalt and molybdenum in cobalt-molybdenum series catalysts generally include impregnation with potassium hydroxide, roasting and water immersion, but using this method, the actual recovery rate of molybdenum is lower than 90%, and sulfuric acid acidification and precipitation The actual recovery rate of molybdenum acid is about 95%, the total recovery rate of molybdenum is less than 85%, the separation of molybdenum is not complete, the quality is not good, and repeated impregnation roasting, energy consumption is high, labor intensity is high, and it is not suitable for popularization and application

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  • Method of recovering molybdenum and cobalt from waste cobalt-molybdenum catalyst

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Embodiment 1

[0031] The method for reclaiming molybdenum and cobalt by the waste cobalt-molybdenum series catalyst described in the application of the present invention comprises the following steps

[0032] 1. Add sodium hydroxide to the spent cobalt-molybdenum-based catalyst at a temperature of 800 °C and roast for 1 hour. The mass ratio of the spent cobalt-molybdenum-based catalyst to the added alkali is 1:5;

[0033] 2. Then wash the roasted product with hot water at 99 ℃, the washing solid-liquid mass ratio is 1:6, the washing time is 1 hour, and then filter;

[0034] 3. Add sulfuric acid to the filtrate to adjust and maintain pH = 6. The reaction temperature is 99 ℃, react for 1 hour, and then filter the solution after the reaction. The filter residue is aluminum hydroxide, and the filtrate is a molybdenum-containing solution. The molybdenum-containing filtrate is adjusted with acid and maintained. pH=2, react at a temperature of 99 °C for 1 hour to obtain molybdic acid precipitation...

Embodiment 2

[0038] Another embodiment of the method described in the application of the present invention adopts the following methods and steps:

[0039] 1. Add sodium carbonate to the spent cobalt-molybdenum-based catalyst at a temperature of 300 °C and roast for 3 hours. The mass ratio of the spent cobalt-molybdenum-based catalyst to the added alkali is 1:3;

[0040]2. Then wash the roasted product with hot water at 60 ℃, the washing solid-liquid mass ratio is 1:2, the washing time is 3 hours, and then filter;

[0041] 3. Add nitric acid to the filtrate to adjust and maintain pH = 8. Reaction temperature is 60 ℃, react for 3 hours, and then filter the solution after reaction. The filter residue is aluminum hydroxide, and the filtrate is molybdenum-containing solution. The molybdenum-containing filtrate is adjusted with acid and maintained pH=0.5, react at a temperature of 60°C for 3 hours to obtain molybdic acid precipitation;

[0042] 4. Wash the obtained molybdic acid precipitate wi...

Embodiment 3

[0046] The method for reclaiming molybdenum-cobalt by the waste cobalt-molybdenum series catalyst described in the application of the present invention adopts the following steps:

[0047] 1. Add calcium hydroxide to the waste cobalt-molybdenum catalyst for roasting at a temperature of 500 °C. The roasting time is 2 hours. The mass ratio of the waste cobalt-molybdenum catalyst to the added alkali is 1:4;

[0048] 2. Then wash the roasted product with hot water at 75 ℃, the washing solid-liquid mass ratio is 1:4, the washing time is 2 hours, and then filter;

[0049] 3. Add hydrochloric acid to the filtrate to adjust and maintain pH = 7. The reaction temperature is 80 ℃, react for 2 hours, and then filter the solution after the reaction. The filter residue is aluminum hydroxide, which is used to recover aluminum. The filtrate is a molybdenum-containing solution, and the molybdenum-containing filtrate Use acid to adjust and maintain pH = 1, react at a temperature of 70 ° C for 2...

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Abstract

The invention provides a method of recovering molybdenum and cobalt from a waste cobalt-molybdenum catalyst. The method comprises the following steps: adding alkali into the waste cobalt-molybdenum catalyst, then roasting the waste catalyst, carrying out washing and filtering, adding an acid into an obtained filtrate to adjust a pH value, filtering a reacted solution, with filter residue being aluminum hydroxide for recovery of aluminum and a filtrate being a molybdenum-containing solution, adjusting the pH value of the molybdenum-containing solution to obtain molybdic acid deposition, washing the molybdic acid deposition with distilled water to wash out impurities adhering on molybdic acid and carrying out roasting so as to obtain molybdenum trioxide; and adding alkali for roasting, drying washed filter residue, introducing carbon monoxide gas after moisture is totally removed and introducing tail gas into a collection container after condensation at the same time, wherein carbonyl cobalt is condensed to form a solid, which allows metal cobalt to be recovered, the tail gas is cyclically used, and reacted filter residue after introduction of carbon monoxide gas can be used for recovery of carriers like magnesium and rare earth. According to the method, used raw materials are cheap, which is beneficial for cost control; steps of the method are simple, so recovery flow of metal cobalt and molybdenum is shortened, and a recovery rate is increased.

Description

technical field [0001] The application of the present invention relates to a method for recovering precious metals, in particular to a method for recovering metal cobalt and molybdenum from waste cobalt-molybdenum catalysts, which belongs to the technical field of resource recovery and environmental protection. Background technique [0002] Cobalt-molybdenum catalysts have outstanding sulfur resistance, and are suitable for ammonia synthesis plants that use coal and heavy oil (or residual oil) as raw materials. without H 2 S or less H 2 In the environment of S, the activity is relatively poor, and it is usually not suitable for ammonia plants that use light oil and natural gas as raw materials. Cobalt-molybdenum-based catalysts usually use the following carrier: Al 2 o 3 、Al 2 o 3 / MgO, this type of catalyst is often added with alkali metal potassium as a co-catalyst to improve its low-temperature activity. When selecting a specific catalyst, not only the activity of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B1/02C22B3/04C22B21/00C22B23/00C22B34/34
CPCY02P10/20
Inventor 王勤苏陶贵陈艳红杨柳
Owner JINGMEN GEM NEW MATERIAL
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