A step-by-step dynamic acid adjustment method for extracting molybdenum

An extraction and dynamic technology, applied in the direction of improving process efficiency, can solve the problems of flowmeter crystallization blockage, affecting extraction operation, long precipitation time, etc., and achieve the effect of eliminating the generation of three-phase substances, reducing the filtration process, and efficiently extracting

Active Publication Date: 2018-09-25
河北欣芮再生资源利用有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the polymerization of monomolybdate ions under acidic conditions to form polymolybdate ions, such as dimolybdate ions (Mo 2 o 7 2- ), trimolybdate ion (Mo 3 o 10 2- ), tetramolybdate ion (Mo 4 o 13 2- ), heptamolybdate ion (Mo 7 o 24 6- ) and octamolybdate ion (Mo 8 o 26 4- ) etc., in the presence of ammonium ions, corresponding ammonium polymolybdate salts are generated, wherein ammonium heptamolybdate is water-soluble, others are slightly soluble in water, and molybdate precipitation is also generated at the same time, and the precipitation time is long. After filtration, the mother liquor Precipitation also continues to occur, causing pumps, pipelines and flowmeters to crystallize and block, emulsification occurs during the extraction process, the extraction agent is lost and the extraction operation is seriously affected

Method used

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  • A step-by-step dynamic acid adjustment method for extracting molybdenum

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Experimental program
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Effect test

Embodiment 1

[0033] This embodiment provides a step-by-step dynamic acid adjustment method for extracting molybdenum, which includes the following steps:

[0034] S101: Mix ammonium sulfate with a waste catalyst solution containing vanadium and molybdenum, and filter after sufficient precipitation to obtain filter residue ammonium metavanadate and filtrate;

[0035] Wherein, the molar ratio of ammonium sulfate and vanadium is 3.5:1, and in the obtained filtrate, the mass concentration of vanadium is 1.51 g / L, the mass concentration of molybdenum is 12.3 g / L, and the pH value is 8.8.

[0036] S102: Use concentrated sulfuric acid with a mass fraction of 92.5% to adjust the pH of the filtrate to 6.8;

[0037] At this time, no precipitation of molybdate (ammonium) occurred, and there was no precipitation after 12 hours.

[0038] S103: Mix the extractant trioctyl tertiary amine, secondary octanol, and sulfonated kerosene uniformly in a volume ratio of 10:10:80 to obtain a tertiary amine-kerosene solution...

Embodiment 2

[0044] This embodiment provides a step-by-step dynamic acid adjustment method for extracting molybdenum, which includes the following steps:

[0045] S101: Mix ammonium sulfate with a waste catalyst solution containing vanadium and molybdenum, and filter after sufficient precipitation to obtain filter residue ammonium metavanadate and filtrate;

[0046] Wherein, the molar ratio of ammonium sulfate and vanadium is 3.2:1, and in the obtained filtrate, the mass concentration of vanadium is 1.8 g / L, the mass concentration of molybdenum is 10.5 g / L, and the pH value is 8.5.

[0047] S102: Use concentrated sulfuric acid with a mass fraction of 92.5% to adjust the pH of the filtrate to 6.5;

[0048] At this time, no precipitation of molybdate (ammonium) occurred, and there was no precipitation after 12 hours.

[0049] S103: Mix the extractant trioctyl tertiary amine, secondary octanol and sulfonated kerosene uniformly in a volume ratio of 10:10:80 to obtain a tertiary amine-kerosene solution; ...

Embodiment 3

[0055] This embodiment provides a step-by-step dynamic acid adjustment method for extracting molybdenum, which includes the following steps:

[0056] S101: Mix ammonium sulfate with a waste catalyst solution containing vanadium and molybdenum, and filter after sufficient precipitation to obtain filter residue ammonium metavanadate and filtrate;

[0057] Wherein, the molar ratio of ammonium sulfate and vanadium is 3.0:1, and in the obtained filtrate: the mass concentration of vanadium is 2.25 g / L, the mass concentration of molybdenum is 8.6 g / L, and the pH value is 9.0.

[0058] S102: Use concentrated sulfuric acid with a mass fraction of 92.5% to adjust the pH of the filtrate to 6.7;

[0059] At this time, no precipitation of molybdate (ammonium) occurred, and there was no precipitation after 12 hours.

[0060] S103: The extractant trioctyl tertiary amine, secondary octanol and sulfonated kerosene are mixed uniformly in a volume ratio of 10:10:80 to obtain a tertiary amine-kerosene solu...

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Abstract

The invention relates to a step-by-step dynamic acid adjustment method for extracting molybdenum, which comprises the following steps: S101: mixing ammonium sulfate with a waste catalyst solution containing vanadium and molybdenum, and filtering after sufficient precipitation to obtain filter residue ammonium metavanadate and filtrate; S102: Use an acid solution to adjust the pH value of the filtrate to 6.5-6.8; S103: use the converted extractant to extract the filtrate treated in S102 to obtain a molybdenum-loaded organic phase and a raffinate aqueous phase; wherein, the extraction is a single-stage three-stage extraction. During the process, the acid solution was added in three sections. The step-by-step dynamic acid adjustment and extraction method for molybdenum provided by the present invention, by adopting the method of adding acid step by step, realizes extraction while adjusting acid, reduces the concentration of molybdenum in the water phase, prevents molybdenum from precipitating during the extraction process, and makes the tertiary amine ‑The kerosene solution extracts molybdenum within the optimum pH value range, so as to realize the efficient extraction of molybdenum, improve the operating conditions, save the amount of sulfuric acid, and increase the recovery rate of molybdenum.

Description

Technical field [0001] The invention relates to the technical field of non-ferrous metal extraction, in particular to a method for extracting molybdenum by stepwise dynamic adjustment of acid. Background technique [0002] The recovery of vanadium and molybdenum from waste catalysts containing molybdenum, vanadium and nickel usually adopts "alkali oxidation roasting-water leaching filtration-filtrate chemical precipitation method for phosphorus removal-purification liquid ammonium salt weak alkaline precipitation-ammonium metavanadate-tertiary amine + kerosene solution acidity The process of extracting molybdenum-sodium hydroxide solution back-extracting molybdenum-concentrated sulfuric acid to precipitate molybdic acid" recovers vanadium and molybdenum. The chemical principle of the separation of vanadium and molybdenum is: under alkaline conditions, ammonium metavanadate has low solubility when ammonium ions are excessive, while ammonium molybdate has high solubility. When usi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/28C22B3/44C22B7/00C22B34/34
CPCC22B3/44C22B7/006C22B34/345C22B3/28Y02P10/20
Inventor 杨双华方金友王金良
Owner 河北欣芮再生资源利用有限公司
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