CN105420505A - Method for separating molybdenum from sulfuric acid precipitation mother liquor obtained in ammonium tetramolybdate preparation - Google Patents

Abstract

The invention belongs to the technical field of wet metallurgy, and specifically relates to a method for separating molybdenum from sulfuric acid precipitation mother liquor obtained in ammonium tetramolybdate preparation, and aims to overcome the shortage of prior art. The provided method can efficiently separate molybdenum from sulfuric acid precipitation mother liquor, recovers molybdenum resource, and provides technical support for the efficient development and utilization of molybdenum resource. A solution extraction method is adopted, N235 is taken as the extraction agent to separate and recover molybdenum from mother liquor, after extraction, the molybdenum loaded organic phase is subjected to back-extraction with ammonia water; and the extraction method is adaptable to the change of molybdenum concentration and is well matched with the technology of extraction method for separating molybdenum. N235 is used to extract molybdenum in sulfuric acid precipitation mother liquor, the molybdenum can be efficiently separated and recycled, and the recovery rate of molybdenum can reach 99% or more. The pH of acid precipitation mother liquor does not need to be adjusted, and thus the reagent cost is saved. The qualified molybdenum back-extraction liquid contains few impurities, does not need a purification treatment, can be directly subjected to acid precipitation to prepare ammonium tetramolybdate, and thus the production cost of ammonium tetramolybdate is largely reduced.

Description

A kind of method from preparing Separation of Molybdenum the heavy mother liquor of ammonium tetramolybdate sulfuric acid acid

Technical field

The invention belongs to technical field of wet metallurgy, being specifically related to a kind of method from preparing Separation of Molybdenum the heavy mother liquor of ammonium tetramolybdate sulfuric acid acid.

Background technology

In ammonium tetramolybdate preparation technology, usually sink operation in acid and can discharge a large amount of mother liquor containing a great deal of molybdenum or waste liquid, ion exchange method, solvent extration, selective precipitation, active carbon adsorption etc. generally can be adopted to realize the Separation and Recovery of molybdenum in mother liquor, but comparatively conventional method mainly ion exchange method and and solvent extration.

Ion exchange method adopts molybdenum in the weak-base ion-exchange resin Separation and Recovery mother liquor of wide aperture usually, saturated resin ammoniacal liquor after absorption or sodium hydroxide solution carry out desorb, resin hydrochloric acid soln after desorb regenerates, after transition, resin carries out drip washing with clear water again, though ion exchange method can realize the recovery of molybdenum in the heavy mother liquor of acid or waste liquid, but complex process, is generally used for the solution of molybdenum concentration in mother liquor or waste liquid lower (being usually less than 2g/L).

Summary of the invention

The object of the invention is to overcome the deficiencies in the prior art, for molybdenum in the heavy mother liquor of sulfuric acid acid, provide a kind of separation and recovery method of efficient molybdenum, the Efficient Development for such Mo resource utilizes and provides technical support.

The present invention is achieved in that

From the method preparing Separation of Molybdenum the heavy mother liquor of ammonium tetramolybdate sulfuric acid acid, specifically comprise the steps:

(1) sink mother liquor to acid directly to extract, extraction agent is volume percent is 7.5%N235+15%TBP+77.5% sulfonated kerosene, before extraction, extraction agent sulfuric acid is made the transition, extraction is carried out in level Four mixer-settler, O/A=2 is compared in operation, duration of contact 3min, extraction temperature 30 ~ 35 DEG C;

(2) control flow check than the stream being than A/O=1 ~ 1.5, molybdenum capacity 12 ~ 15g/L in proof load organic phase, in raffinate aqueous phase, molybdenum content is lower than 50mg/L;

(3) load organic phases is with 150g/L ammoniacal liquor as strippant, strips and to carry out in level Four mixer-settler, and operation compares A/O=3, two-phase 5min duration of contact, and in anti-stripping agent, molybdenum concentration is about 130g/L;

(4) molybdenum anti-stripping agent delivers to purification and the heavy operation of acid prepares ammonium tetramolybdate or many ammonium molybdates product.

The invention has the beneficial effects as follows:

Solution extraction of the present invention adopts N235 as molybdenum in extraction agent Separation and Recovery mother liquor, after extraction, molybdenum load organic phases ammoniacal liquor is stripped, extraction process has stronger adaptability to molybdenum concentration change in mother liquor, and can realize being connected preferably with adopting the technique of extraction process Separation of Molybdenum.The high efficiency separation that the N235 molybdenum extracted in the heavy mother liquor of sulfuric acid acid can realize molybdenum reclaims, and molybdenum recovery can reach more than 99%; The heavy mother liquor of acid, without the need to regulating pH, saves reagent cost; Molybdenum reextraction qualifying liquid impurity is few, without the need to purifying treatment, directly can carry out that acid is heavy prepares ammonium tetramolybdate, considerably reduce ammonium tetramolybdate production cost.

Accompanying drawing explanation

Fig. 1 is a kind of schema of method from preparing Separation of Molybdenum the heavy mother liquor of ammonium tetramolybdate sulfuric acid acid of the present invention.

Embodiment

Below in conjunction with drawings and Examples, the present invention is described further.

Embodiment 1

Heavy mother liquor: ρ (Mo) 11.3g/L, pH2.5, ρ (As) 5mg/L, ρ (P) 6mg/L, ρ (Si) 5mg/L, the ρ (SO of acid ₄ ^2-) 202g/L.

Extraction molybdenum organic phase: 7.5%N235+15%TBP+77.5% sulfonated kerosene

Extracting operation condition: compare: O/A=2, flows than A/O=1.2, duration of contact 3min, extraction temperature 32 DEG C

Molybdenum load organic phases: ρ (Mo) ~ 13.5g/L

Molybdenum raffinate aqueous phase: ρ (Mo) <45mg/L

Strippant: 150g/L ammoniacal liquor

Reextraction molybdenum operational condition: compare: A/O=3, flows than O/A=10, duration of contact 5min

Molybdenum anti-stripping agent: ρ (Mo) ~ 130g/L

Embodiment 2

Heavy mother liquor: ρ (Mo) 14.8g/L, pH2.14, ρ (As) 6mg/L, ρ (P) 2mg/L, ρ (Si) 5mg/L, the ρ (SO of acid ₄ ^2-) 210.8g/L.

Extraction molybdenum organic phase: 7.5%N235+15%TBP+77.5% sulfonated kerosene

Extracting operation condition: compare: O/A=2, flows than A/O=1, duration of contact 3min, extraction temperature 30 DEG C

Molybdenum load organic phases: ρ (Mo) ~ 14.5g/L

Molybdenum raffinate aqueous phase: ρ (Mo) <50mg/L

Strippant: 150g/L ammoniacal liquor

Reextraction molybdenum operational condition: compare: A/O=3, flows than O/A=9, duration of contact 5min

Molybdenum anti-stripping agent: ρ (Mo) ~ 130g/L

Embodiment 3

Heavy mother liquor: ρ (Mo) 10.9g/L, pH2.01, ρ (As) 15mg/L, ρ (P) 4mg/L, ρ (Si) 6mg/L, the ρ (SO of acid ₄ ^2-) 207.9g/L

Extraction molybdenum organic phase: 7.5%N235+15%TBP+77.5% sulfonated kerosene

Extracting operation condition: compare: O/A=2, flows than A/O=1.2, duration of contact 3min, extraction temperature 34 DEG C

Molybdenum load organic phases: ρ (Mo) ~ 13g/L

Molybdenum raffinate aqueous phase: ρ (Mo) <50mg/L

Strippant: 150g/L ammoniacal liquor

Reextraction molybdenum operational condition: compare: A/O=3, flows than O/A=10, duration of contact 5min

Molybdenum anti-stripping agent: ρ (Mo) ~ 130g/L

Embodiment 4

Heavy mother liquor: ρ (Mo) 8.9g/L, pH2.23, ρ (As) 10mg/L, ρ (P) 4mg/L, ρ (Si) 5mg/L, the ρ (SO of acid ₄ ^2-) 217.9g/L

Extraction molybdenum organic phase: 7.5%N235+15%TBP+77.5% sulfonated kerosene

Extracting operation condition: compare: O/A=2, flows than A/O=1.5, duration of contact 3min, extraction temperature 35 DEG C

Molybdenum load organic phases: ρ (Mo) ~ 13.3g/L

Molybdenum raffinate aqueous phase: ρ (Mo) <40mg/L

Strippant: 150g/L ammoniacal liquor

Reextraction molybdenum operational condition: compare: A/O=3, flows than O/A=10, duration of contact 5min

Molybdenum anti-stripping agent: ρ (Mo) ~ 130g/L

Above embodiments of the invention are explained in detail, above-mentioned embodiment is only optimum embodiment of the present invention, but the present invention is not limited to above-described embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.

Claims (1)

1., from the method preparing Separation of Molybdenum the heavy mother liquor of ammonium tetramolybdate sulfuric acid acid, specifically comprise the steps:

(1) sink mother liquor to acid directly to extract, extraction agent is volume percent is 7.5%N235+15%TBP+77.5% sulfonated kerosene, before extraction, extraction agent sulfuric acid is made the transition, extraction is carried out in level Four mixer-settler, O/A=2 is compared in operation, duration of contact 3min, extraction temperature 30 ~ 35 DEG C;

(2) control flow check than the stream being than A/O=1 ~ 1.5, molybdenum capacity 12 ~ 15g/L in proof load organic phase, in raffinate aqueous phase, molybdenum content is lower than 50mg/L;

(3) load organic phases is with 150g/L ammoniacal liquor as strippant, strips and to carry out in level Four mixer-settler, and operation compares A/O=3, two-phase 5min duration of contact, and in anti-stripping agent, molybdenum concentration is about 130g/L;

(4) molybdenum anti-stripping agent delivers to purification and the heavy operation of acid prepares ammonium tetramolybdate or many ammonium molybdates product.