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Method for extracting molybdenum by sub-step dynamic acid adjustment

An extraction and dynamic technology, applied in the direction of improving process efficiency, etc., can solve problems such as flow meter crystallization blockage, affect extraction operation, and produce emulsion, and achieve the effect of eliminating the generation of three-phase matter, reducing the filtration process, and smooth transportation

Active Publication Date: 2017-07-25
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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  • Method for extracting molybdenum by sub-step dynamic acid adjustment

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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, comprising the following steps:

[0034] S101: mixing ammonium sulfate with the vanadium-molybdenum-containing waste catalyst solution, and filtering 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 1.51g / L, the mass concentration of molybdenum is 12.3g / L, and the pH value is 8.8.

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

[0037] At this time, molybdic acid (ammonium) precipitation did not occur, and there was still no precipitation after standing for 12 hours.

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

Embodiment 2

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

[0045] S101: mixing ammonium sulfate with the vanadium-molybdenum-containing waste catalyst solution, and filtering 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 1.8g / L, the mass concentration of molybdenum is 10.5g / L, and the pH value is 8.5.

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

[0048] At this time, molybdic acid (ammonium) precipitation did not occur, and there was still no precipitation after standing for 12 hours.

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

Embodiment 3

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

[0056] S101: mixing ammonium sulfate with the vanadium-molybdenum-containing waste catalyst solution, and filtering 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 2.25g / L, the mass concentration of molybdenum is 8.6g / L, and the pH value is 9.0.

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

[0059] At this time, molybdic acid (ammonium) precipitation did not occur, and there was still no precipitation after standing for 12 hours.

[0060] S103: Mix the extractant trioctyl tertiary amine, secondary octanol and sulfonated kerosene in a volume ratio of 10:10:80 to obtain a terti...

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Abstract

The invention relates to a method for extracting molybdenum by sub-step dynamic acid adjustment. The method comprises the following steps: (S101) ammonium sulfate and vanadium and molybdenum-contained waste catalyst solution are mixed, and are filtered after full precipitation to obtain residues-ammonium metavanadate and filtrates; (S102) the pH value of the filtrates is adjusted to 6.5-6.8 by acid solution; and (S103) a transformed extracting agent is adopted to extract the filtrates treated in the step (S102) to obtain a molybdenum-loaded organic phase and a raffinate water phase, wherein the extraction is single-grade three-section extraction; and in the extracting process, the acid solution is respectively fed by three stages. The method for extracting molybdenum by sub-step dynamic acid adjustment realizes adjustment of acid during extracting through a sub-step acid feeding method to reduce the concentration of molybdenum in the water phase, so that the molybdenum is not precipitated in the extracting process, the molybdenum is extracted in an optimal pH value range by tertiary amine-kerosene solution, the high-efficiency molybdenum extraction is realized, the operation conditions are improved, the consumption of sulfuric acid is saved, and the molybdenum recovery rate is increased.

Description

technical field [0001] The invention relates to the technical field of non-ferrous metal extraction, in particular to a step-by-step dynamic acid adjustment method for extracting molybdenum. Background technique [0002] To recover vanadium and molybdenum from molybdenum-containing vanadium-nickel waste catalyst, usually adopt "alkali oxidation roasting - water immersion filtration - filtrate chemical precipitation method to remove phosphorus - purification liquid ammonium salt weak alkaline precipitation ammonium metavanadate - tertiary amine + kerosene solution acidic The process of extracting molybdenum-sodium hydroxide solution back-extracting molybdenum-concentrated sulfuric acid to precipitate molybdenum acid can recover vanadium and molybdenum. The chemical principle of the separation of vanadium and molybdenum is: under alkaline conditions, the solubility of ammonium metavanadate is small when ammonium ions are excessive, while the solubility of ammonium molybdate is...

Claims

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Application Information

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Patent Type & Authority Applications(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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