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Method for recycling high purity molybdenum from molybdenum-containing spent catalyst

A technology of waste catalyst and soda ash, applied in the direction of improving process efficiency, can solve the problems of difficult to completely remove, pollute the environment, low recovery rate of molybdenum, etc., and achieve the effect of low cost, low risk and improved purity

Active Publication Date: 2009-05-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since sulfur-containing compounds are usually adsorbed on the spent catalyst, sulfur dioxide will be produced while removing the oil of the spent catalyst by high temperature, so there is a problem of polluting the environment
[0005] In addition, in the above-mentioned methods, the waste materials containing molybdenum are all subjected to high-temperature treatment. For catalysts deactivated by carbon deposition, especially spent catalysts with a large amount of carbon deposition, due to the concentrated heat release during high-temperature calcination and improper temperature control, It will make it difficult to completely remove the carbon deposit attached to the catalyst, and then carry out conventional leaching, which will inevitably lead to low recovery rate of molybdenum

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 10.0g contains 16w% MoO 3 Industrial MoO 3 / Alumina waste catalyst, after being pulverized to 120 mesh, fully mixed with 10g of soda ash and 5g of magnesium oxide, kept at 70°C for 2 hours, and adjusted the oxygen content to 5.0v%; at 240°C for 2 hours, adjusted the oxygen content Gradually increase to 12.0v%, keep the temperature at 430°C for 2 hours, gradually increase the oxygen content to 18.0v%; keep the temperature at 530°C for 2 hours, gradually increase the oxygen content to 21v%. The heating rate was 5°C per minute. After cooling, soak in water at 80°C for 2h, filter and wash the precipitate fully, and separate. The pH of the filtrate was adjusted to 8.5 with concentrated sulfuric acid, and then filtered; the pH of the filtrate was adjusted to 1.2 with nitric acid to precipitate molybdenum acid, and then separated by filtration. Add molybdic acid to ammonia water to dissolve, then adjust the pH value to 3.0 with nitric acid to precipitate ammonium molybdate,...

Embodiment 2

[0033] 10.0g contains 20w% MoO 3 Industrial MoO 3 / alumina-silica waste catalyst, crushed to 120 mesh, fully mixed with 15g of sodium potassium carbonate and 5g of magnesium oxide, kept at 70°C for 2 hours, and adjusted the oxygen content to 5.0v%; kept at 240°C for 2 hours Hours, gradually increase the oxygen content to 12.0v%, keep the temperature at 430°C for 2 hours, gradually increase the oxygen content to 18.0v%; keep the temperature at 540°C for 2 hours, gradually increase the oxygen content to 21v%, The heating rate between each section is 8°C per minute. After cooling, soak in water at 70°C for 3 hours, filter and fully wash the precipitate, and separate. The filtrate was first adjusted to pH 8.5 with concentrated sulfuric acid, and then filtered; MgSO with a liquid-solid ratio (weight ratio) of 10:1 was added to the filtrate 4 , Stir for 1h, filter; then adjust the pH of the filtrate to 1.2 with nitric acid to precipitate molybdic acid, and separate by filtration. ...

Embodiment 3

[0035] 10.0g contains 24w% MoO 3 Industrial MoO 3 / alumina-silicon oxide waste catalyst, after pulverizing to 150 mesh, directly mixes fully with sodium hydroxide and magnesium oxide (sodium hydroxide 5g, magnesium oxide is 5g). Keep the temperature at 70°C for 1 hour, adjust the oxygen content to 5.0v%,; keep the temperature at 250°C for 2 hours, gradually increase the oxygen content to 12.0v%, and keep the temperature at 450°C for 2 hours, gradually increase the oxygen content It is 18.0v%; keep the temperature at 550°C for 3 hours, gradually increase the oxygen content to 21v%, and the temperature rise rate between each stage is 5°C per minute. After cooling, add 40mL of water for leaching, and stir at 90°C for 3h. Filter and wash the precipitate well and separate. The filtrate was first adjusted to pH 9.0 with concentrated sulfuric acid, and filtered; the liquid-solid ratio (weight ratio) was added to the filtrate with Mg(NO 3 ) 2 , Stir for 1h, filter; then adjust th...

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Abstract

The invention discloses a method for recovering molybdenum from waste catalyst containing molybdenum. The method mainly comprises the following steps of: carrying out pretreatment to the waste catalyst containing molybdenum, leaching the molybdenum into the solution, and purifying and recovering the molybdenum from the solution; wherein, the pretreatment carried out to the waste catalyst containing molybdenum is as follows: the crushed waste catalyst containing molybdenum, alkaline matters and magnesium oxide are mixed fully by proper proportion, and then high temperature roasting treatment is carried out. The treatment method has simple operation, low cost, little pollution, little hazard, low requirements on equipment and easy industrialization; and the adding proportion of the alkaline matters and magnesium oxide is proper, thus being capable of absorbing harmful substances released when the waste catalyst is roasted; in addition, the adding of the proper magnesium oxide can lead the waste catalyst to keep loose state, avoids the phenomenon that the waste catalyst containing oil is roasted directly to lead partial temperature to be overhigh, which then causes the sublimation of the molybdenum and further causes the recovery rate to be reduced, thus improving the recovery rate of the molybdenum.

Description

1. Technical field [0001] The invention relates to a method for recovering high-purity molybdenum-containing compounds from molybdenum-containing waste catalysts, in particular to a method for recovering molybdenum from molybdenum-containing waste catalysts. 2. Background technology [0002] With the development of industry, the advancement of science and technology, and the improvement of environmental regulations, the demand for petroleum and petrochemical products is increasing day by day, and the amount of catalysts used to produce various products is also increasing. Molybdenum series catalysts are characterized by their superior catalytic performance. Favored by the world, this series of catalysts has been widely used in various industries. At the same time, due to the relative shortage of molybdenum metal resources, there is also a large demand in the fields of national defense and steel, which has caused the price of molybdenum metal to soar at home and abroad. Ther...

Claims

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Application Information

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IPC IPC(8): C22B34/34C22B1/14C22B1/02C22B3/04
CPCY02P10/20
Inventor 王敏凌凤香张喜文孙万付
Owner CHINA PETROLEUM & CHEM CORP
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