CN113512644B - Method for separating rhenium from ammonium molybdate solution - Google Patents

Method for separating rhenium from ammonium molybdate solution Download PDF

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CN113512644B
CN113512644B CN202111072052.6A CN202111072052A CN113512644B CN 113512644 B CN113512644 B CN 113512644B CN 202111072052 A CN202111072052 A CN 202111072052A CN 113512644 B CN113512644 B CN 113512644B
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rhenium
nanofiltration
ammonium molybdate
molybdenum
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CN113512644A (en
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蒋国民
雷吟春
孟云
刘陈
王凯
刘永丰
闫虎祥
赵次娴
廖圆
齐伟
岑家山
高伟荣
陈龙
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Science Environmental Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/34—Obtaining molybdenum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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Abstract

The invention discloses a method for separating rhenium from an ammonium molybdate solution. Firstly, carrying out primary nanofiltration on ammonium molybdate liquid, and separating molybdenum-rich liquid and primary permeate liquid; adding the hydroximic acid salt solution into the primary permeate liquid, stirring, adding inorganic acid to adjust the pH to 0.5-2.0, adding hydrogen peroxide, and reacting at room temperature for 30-60 min to obtain a complex solution, wherein the hydroximic acid salt: hydrogen peroxide: mo molar ratio = (2-4): (0.1-1.0): 1; carrying out secondary nanofiltration on the complex solution to separate out secondary concentrated solution and rhenium-rich solution 1; and (3) carrying out nanofiltration on the secondary concentrated solution for three times, and separating out a tertiary concentrated solution and a rhenium-rich solution 2. The obtained rhenium-rich liquid contains Mo less than 0.01mg/L and Re/Mo more than 2X 104. Compared with the ammonium molybdate solution, the volume of the obtained molybdenum-rich liquid phase is reduced by more than 1 time, the molybdenum concentration is improved by more than 2 times, the Mo loss rate is less than 0.01 percent, and the energy consumption and the reagent consumption are reduced for the subsequent resource utilization of molybdenum.

Description

Method for separating rhenium from ammonium molybdate solution
Technical Field
The invention relates to the field of metal separation, in particular to a method for separating rhenium from an ammonium molybdate solution.
Background
Rhenium is a rare metal and is often associated with molybdenum ore, so that rhenium and molybdenum are often separated from the solution in molybdenum smelting. The separation of rhenium and molybdenum is divided into two modes of firstly extracting rhenium and firstly extracting molybdenum.
Firstly, extract rhenium
(1) Extraction and ion exchange process
MoO at pH < 12 2+The cation has absolute dominance in the solution, and SO in the solution4 2-At higher concentrations molybdenum will form MoO2（SO4）2 -. Re in ReO under acidic conditions4 -The form exists, and an amine extractant or a weakly basic resin ReO is adopted4 -Can be superior to MoO2 2+And MoO2（SO4）2 -Is extracted or adsorbed first. CN106367599A discloses a method for extracting rhenium from molybdenum smelting flue gas, which is carried out in SO4 2-And preferably extracting rhenium by adopting trialkylamine under the condition of 80-100 g/L. Preferential extraction of H from solution requiring rhenium under acidic conditions2SO4The concentration is more than or equal to 80g/L, and the molybdenum has 5-10% co-extraction loss.
When the pH value is more than 6, the molybdenum is MoO4 2-Form exists, ReO4 -The affinity with the resin is much higher than that of MoO4 2-And OH-The strong alkaline resin can preferentially adsorb rhenium, but an oxidant is required to be added during desorption, so that the resin is very destructive. The method comprises the steps of firstly adjusting the pH of molybdenite concentrate alkaline pressure boiling liquid to 7.5-10, and then extracting rhenium by using a 2-5% primary amine-30-50% neutral phosphate-kerosene system. The method has the advantages that the organic phase accounts for a large proportion of phosphate and the loss is large during extraction.
(2) Precipitation method
Methyl violet can be from pH 8EAnd rhenium is selectively precipitated in the 8.5 solution, molybdenum is left in the mother solution, but the precipitation rate of rhenium is only 91-97%, the reuse rate of methyl violet is only 90-95%, and the use efficiency is low. KCl can be reacted with ReO4 -Binding to form very low solubility KReO4Cooling and crystallizing to obtain KReO4Crystal, but the method requires that the Re concentration in the solution is more than or equal to 10g/L, otherwise, the rhenium precipitation rate is lower.
(3) Activated carbon adsorption or flotation process
The activated carbon can adsorb rhenium, but the rhenium adsorption rate can be more than 80% only in the range of pH = 2.0-5.2 or 8.2-10.6, and molybdenum is also partially adsorbed. CN110777270A discloses a method for selective flotation separation of molybdenum-rhenium acid radicals in alkaline leachate, which comprises the steps of adjusting the pH value of alkaline leachate containing molybdenum acid radicals and rhenate radicals to 7.1-12, adding an organic modified activated carbon collecting agent and a surfactant, wherein the collecting agent and the surfactant are composed of triethylene tetramine, tetraethylene pentamine, methyl violet 10B and cocamidopropyl betaine, and performing air flotation, wherein a foam product is a rhenium-rich component, and the residual liquid is a molybdenum-rich solution. Activated carbon is used for adsorption or flotation, the recovery rate is only 80-96% when rhenium is desorbed, and the loss is large.
Second, firstly extracting molybdenum
(1) Extraction process
At pH < 2.5 the molybdenum fraction is in MoO2 2+The form exists, and MoO can be preferentially extracted by adopting P204 and Kelex100 type extractants2 2 +. CN109055747A discloses a method for extracting and separating molybdenum and rhenium under an acidic condition, wherein a neutral phosphorus extractant, a tertiary amine or quaternary ammonium salt compound extractant are adopted to preferentially extract molybdenum under the pH value of 1.5-4.5, wherein the phosphorus extractant occupies 30-50% of the volume of an organic phase, and the loss is large during extraction.
(2) Ion exchange process
CN109179506A discloses a method for synergistically recovering rhenium and molybdenum from molybdenum concentrate roasting leacheate, the method pretreats the solution and adjusts the pH value to 0.2-1.5, rhenium is adsorbed by composite amino ethylene macroporous weak base type anion exchange resin, molybdenum is adsorbed by tertiary amino acrylic acid macroporous weak base type anion exchange resin, rhenium is not lost, but the loss rate of molybdenum is only controlled to be less than 8%.
(2) Precipitation method
Using MoO4 2-Is easy to react with Fe3+And Ca2+Precipitates are generated, and molybdenum is precipitated firstly due to the characteristic of higher solubility of the rhenate. CN101050489A discloses a method for separating and extracting rhenium and co-producing a molybdenum-iron alloy from a rhenium-molybdenum mixed solution, wherein a ferric salt and an organic carboxylic acid compound and/or an organic carboxylic acid are added into the rhenium-molybdenum mixed solution at the pH of 4-6 to precipitate molybdenum. But about 2-5% of rhenium is lost when molybdenum is precipitated.
Besides the above methods, there are liquid membrane method, extraction method, electrodialysis method, etc., but these methods are still under study and have some distance from industrial application. In the common molybdenum-rhenium separation method, an extraction method and an ion exchange method are adopted, and about 1-5% of loss is caused in the process of using an extracting agent and resin; the precipitation method has low precipitation efficiency, and the product can carry impurities; the active carbon adsorption or flotation method has low metal recovery rate and the active carbon is easy to inactivate. The purpose of these methods is to separate a certain metal completely at a time, which results in greater process throughput and greater losses; when one metal is separated, the concentration of the other metal in the solution is almost unchanged, and concentration needs to be continuously concentrated subsequently.
Disclosure of Invention
The technical problem solved by the invention is as follows: aiming at the problem of the existing rhenium and molybdenum separation method, the method capable of synchronously improving the molybdenum concentration and reducing the molybdenum solution treatment capacity during rhenium and molybdenum separation is provided.
The invention is realized by adopting the following technical scheme:
a method for separating rhenium from an ammonium molybdate solution, comprising the steps of:
carrying out primary nanofiltration on ammonium molybdate liquid, and separating molybdenum-rich liquid and primary permeate liquid;
and (2) adding a hydroximic acid salt solution into the primary permeate, stirring for 5-10 min, adding an inorganic acid to adjust the pH to 0.5-2.0, and then adding hydrogen peroxide to react for 30-60 min at room temperature to obtain a complex solution. Wherein the hydroxamate salt: hydrogen peroxide: mo molar ratio = (2-4): (0.1-1.0): 1.
step (3), carrying out secondary nanofiltration on the complex solution, and separating out a secondary concentrated solution and a rhenium-rich solution 1;
and (4) carrying out nanofiltration on the secondary concentrated solution for three times, and separating out a tertiary concentrated solution and a rhenium-rich solution 2.
In the method for separating rhenium from the ammonium molybdate solution, in the step (1), the concentration of Re in the ammonium molybdate solution is 0.05-5 g/L, and the concentration of Mo in the ammonium molybdate solution is 1-10 g/L.
In the method for separating rhenium from the ammonium molybdate solution, in particular, in the step (1), the step (2) and the step (3), the membrane adopted for nanofiltration has a molecular weight cutoff of 150-300 daltons, an operating pressure of 0.5-3.5 MPa and a temperature of 20-50 ℃.
In the method for separating rhenium from the ammonium molybdate solution, specifically, in the step (1), the nanofiltration is intermittent operation, the molybdenum-rich solution is subjected to circulating nanofiltration, and the nanofiltration is stopped when the volume of the primary permeate is controlled to be 50-60% of that of the ammonium molybdate solution.
In the method for separating rhenium from the ammonium molybdate solution, in particular, in the step (2), the hydroxamate is one or more of octyl hydroxamate ammonium salt, salicyl hydroxamate ammonium salt and acetyl hydroxamate ammonium salt.
In the method for separating rhenium from the ammonium molybdate solution, specifically, in the step (3), the nanofiltration is intermittent operation, the secondary concentrated solution is subjected to circulating nanofiltration, and the nanofiltration is stopped when the volume of the rhenium-rich solution 1 is controlled to be 60-80% of the volume of the complex solution.
In the method for separating rhenium from the ammonium molybdate solution, specifically, in the step (4), the nanofiltration is performed intermittently, the third concentrated solution is subjected to circulating nanofiltration, and the nanofiltration is stopped when the volume of the rhenium-rich solution 2 is controlled to be 60-80% of that of the second concentrated solution.
The method for separating rhenium from the ammonium molybdate solution has the following beneficial effects:
(1) the invention utilizes hydroximic acid salt, hydrogen peroxide and molybdenum to complex into macromolecules which can be intercepted by a nanofiltration membrane and ReO4 -Can penetrate throughThe nano filter membrane is characterized by carrying out deep separation on rhenium. According to the pH and the concentration range of Re and Mo, the hydroximic acid salt is determined: hydrogen peroxide: the preparation proportion of the Mo molar ratio is favorable for saving energy consumption, reducing reagent consumption and reducing the complicated flow caused by reagent recovery. The donor atom of the hydroxamate is N or O, which can provide a lone pair of electrons and MoO2 2+And (4) complexing. Hydroximes and MoO at pH 1.0-2.02 2+The complexing ability of the catalyst is stronger than that of pH0.5-1.0, so that the addition of hydrogen peroxide can be correspondingly reduced. Mo in the final rhenium-rich liquid is less than 0.01mg/L, Re/Mo is more than 2X 104The rhenium can be directly precipitated, concentrated and crystallized, extracted or ion exchanged to recover the rhenium. Compared with the original ammonium molybdate solution, the volume of the obtained molybdenum-rich liquid phase is reduced by more than 1 time, the molybdenum concentration is improved by more than 2 times, the Mo loss rate is less than 0.01 percent, and the equipment investment and the occupied area are reduced for the subsequent resource utilization of molybdenum.
(2) The method adopts hydroximic acid salt and hydrogen peroxide to coordinate molybdenum, has the defect that the reaction needs more than 24 hours compared with the traditional single hydrogen peroxide complexing method, and has the advantage of short reaction time.
(3) The nanofiltration of the invention adopts intermittent operation, the molybdenum concentration in the molybdenum-rich liquid and the concentrated solution is improved by controlling the volume of the solution of the permeate liquid, and compared with the continuous operation mode of controlling the flux of the membrane, the molybdenum concentration can be improved to the maximum extent while the smooth operation of the nanofiltration is ensured.
The invention is further described with reference to the following figures and detailed description.
Drawings
FIG. 1 is a process flow diagram for molybdenum-rhenium separation according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way.
Example 1: 5000mL of ammonia water back extraction liquid after molybdenum and rhenium are co-extracted by molybdenum smelting flue ash leacheate, and Mo5159mg/L, Re218 mg/L. The ammonium molybdate solution is subjected to one nanofiltration to obtain 2500mL of molybdenum-rich solution and Mo10297mg/L, Re174mg/L, wherein the Mo concentration is improved by 2 times, and the Mo/Re is improved by 2.5 times; obtaining 2500mL of primary permeate,Mo21mg/L, Re262 mg/L. Adding 10g of 2% salicylhydroxamic acid ammonium salt solution into the primary permeate, stirring for 5min, adding sulfuric acid to adjust the pH to 1.2, adding 0.03mL of 30% hydrogen peroxide, and reacting at room temperature for 30min to obtain a complex solution. The complex solution is subjected to secondary nanofiltration to obtain 1500mL rhenium-rich solution 1, wherein Mo is less than 0.01mg/L, Re316 mg/L; 1000mL of secondary concentrated solution and Mo52mg/L, Re181mg/L are obtained. Carrying out nanofiltration on the secondary concentrated solution for three times to obtain 600mL of rhenium-rich solution 2, wherein Mo is less than 0.01mg/L, Re195 mg/L; 400mL of the third concentrated solution and Mo131mg/L, Re160mg/L of the third concentrated solution are obtained. The third concentrated solution is mixed into the ammonium molybdate solution and enters the main flow. The total volume of the mixed rhenium-rich liquid 1 and the rhenium-rich liquid 2 is 2100mL, Mo is less than 0.01mg/L, Re281mg/L, and Re/Mo is more than 2.81 multiplied by 104The pure ammonium perrhenate can be prepared by removing precipitation, concentration crystallization, extraction or ion exchange.
Example 2: 5000mL of ammonia water back extraction liquid after molybdenum and rhenium are co-extracted by molybdenum smelting flue ash leacheate, and Mo5159mg/L, Re218 mg/L. The ammonium molybdate solution is subjected to one-time nanofiltration to obtain 2000mL of molybdenum-rich solution and Mo12860mg/L, Re149mg/L, wherein the Mo concentration is improved by 2.5 times, and the Mo/Re is improved by 3.7 times; 3000mL of primary permeate and Mo25mg/L, Re264mg/L of primary permeate were obtained. Adding 20g of 2% octyl hydroximic acid ammonium salt solution into the primary permeate, stirring for 8min, adding sulfuric acid to adjust the pH to 0.8, adding 0.07mL of 30% hydrogen peroxide, and reacting at room temperature for 40min to obtain a complex solution. Carrying out secondary nanofiltration on the complex solution to obtain 2100mL rhenium-rich solution 1, wherein Mo is less than 0.01mg/L, Re282 mg/L; 900mL of secondary concentrated solution and Mo83mg/L, Re222mg/L are obtained. Performing nanofiltration on the secondary concentrated solution for three times to obtain 630mL rhenium-rich solution 2, wherein Mo is less than 0.01mg/L, Re234 mg/L; 270mL of the third concentrated solution and Mo278mg/L, Re194mg/L are obtained. The third concentrated solution is mixed into the ammonium molybdate solution and enters the main flow. 2730mL of mixed rhenium-rich liquid 1 and rhenium-rich liquid 2, Mo is less than 0.01mg/L, Re271mg/L, and Re/Mo is more than 2.71 multiplied by 104The pure ammonium perrhenate can be prepared by removing precipitation, concentration crystallization, extraction or ion exchange.
Example 3: 5000mL of ammonia water back extraction liquid after molybdenum and rhenium are co-extracted by the molybdenum calcine nitric acid pre-leaching solution, and Mo7128mg/L, Re414 mg/L. The ammonium molybdate solution is subjected to one nanofiltration to obtain 2000mL of molybdenum-rich solution and 2.5 times of Mo concentration and 2.9 times of Mo/Re concentration, wherein the Mo17778mg/L, Re357mg/L is obtained; 3000mL of primary permeate and Mo28mg/L, Re452mg/L of primary permeate were obtained. 16g of 2% ammonium acetylhydroxamate solution was added to the first permeate, and the mixture was stirred for 10min, adding sulfuric acid to adjust the pH value to 1.8, adding 0.05mL of 30% hydrogen peroxide, and reacting at room temperature for 60min to obtain a complexing solution. Carrying out secondary nanofiltration on the complex solution to obtain 2100mL rhenium-rich solution 1, wherein Mo is less than 0.01mg/L, Re476 mg/L; obtain 900mL of secondary concentrated solution and Mo93mg/L, Re396 mg/L. Performing nanofiltration on the secondary concentrated solution for three times to obtain 630mL rhenium-rich solution 2, wherein Mo is less than 0.01mg/L, Re411 mg/L; 270mL of the third concentrated solution and Mo311mg/L, Re361mg/L are obtained. The third concentrated solution is mixed into the ammonium molybdate solution and enters the main flow. The total volume of 2730mL of the mixed rhenium-rich liquid 1 and the rhenium-rich liquid 2 is less than 0.01mg/L, Re461mg/L, and the Re/Mo is more than 4.61 multiplied by 104The pure ammonium perrhenate can be prepared by removing precipitation, concentration crystallization, extraction or ion exchange.
Referring to the following table, the rhenium-rich liquids obtained in examples 1, 2 and 3 had Mo < 0.01mg/L and Re/Mo > 2X 104(ii) a Compared with the ammonium molybdate solution, the volume of the obtained molybdenum-rich liquid phase is reduced by more than 1 time, the molybdenum concentration is improved by more than 2 times, the Mo loss rate is less than 0.01 percent, and the energy consumption and the reagent consumption are reduced for the subsequent resource utilization of molybdenum.
TABLE rhenium isolation effectiveness in example 1
Figure 970028DEST_PATH_IMAGE002
TABLE rhenium isolation effectiveness in example 2
Figure 418327DEST_PATH_IMAGE004
TABLE rhenium isolation effectiveness in example 3
Figure 604589DEST_PATH_IMAGE006

Claims (8)

1. A method for separating rhenium from an ammonium molybdate solution, characterized by the steps of:
(1) carrying out primary nanofiltration on the ammonium molybdate liquid, and separating a molybdenum-rich liquid and a primary permeate;
(2) adding a hydroximic acid salt solution into the primary permeate, stirring for 5-10 min, adding an inorganic acid to adjust the pH to 0.5-2.0, adding hydrogen peroxide, and reacting at room temperature for 30-60 min to obtain a complex solution, wherein the hydroximic acid salt: hydrogen peroxide: mo molar ratio = (2-4): (0.1-1.0): 1;
(3) carrying out secondary nanofiltration on the complex solution to separate out a secondary concentrated solution and a rhenium-rich solution 1;
(4) carrying out nanofiltration on the secondary concentrated solution for three times, and separating out a tertiary concentrated solution and a rhenium-rich solution 2;
in the nanofiltration in the step (1), the step (2) and the step (3), the molecular weight cut-off of the adopted membrane is 150-300 daltons.
2. The method for separating rhenium from the ammonium molybdate solution according to the claim 1, wherein in the step (1), the concentration of Re in the ammonium molybdate solution is 0.05 to 5g/L, and the concentration of Mo in the ammonium molybdate solution is 1 to 10 g/L.
3. The method for separating rhenium from an ammonium molybdate solution as claimed in claim 1, wherein the inorganic acid is adjusted to a pH value in the range of 1.0 to 2.0, and the ratio of the hydroxamate: hydrogen peroxide: mo molar ratio = (2-4): (0.1-0.5): 1; when the pH value is adjusted to be 0.5-1.0 by inorganic acid, the content of hydroximic acid salt is as follows: hydrogen peroxide: mo molar ratio = (2-4): (0.5-1.0): 1.
4. the method for separating rhenium from an ammonium molybdate solution according to claim 1, wherein the nanofiltration in the steps (1), (2) and (3) is performed at an operating pressure of 0.5-3.5 MPa and a temperature of 20-50 ℃.
5. The method for separating rhenium from the ammonium molybdate solution according to the claim 1, wherein the nanofiltration in the step (1) is a batch operation, the molybdenum-rich solution is subjected to circulating nanofiltration, and the nanofiltration is stopped when the volume of the primary permeate is controlled to be 50-60% of the volume of the ammonium molybdate solution.
6. The method for separating rhenium from an ammonium molybdate solution as claimed in claim 1, wherein in the step (2), the hydroxamate is one or more of octyl hydroxamate ammonium salt, salicyl hydroxamate ammonium salt and acetyl hydroxamate ammonium salt.
7. The method for separating rhenium from an ammonium molybdate solution as claimed in claim 1, wherein in the step (3), the nanofiltration is performed intermittently, the secondary concentrated solution is subjected to circulating nanofiltration, and the nanofiltration is stopped when the volume of the rhenium-rich solution 1 is controlled to be 60-80% of the volume of the complex solution.
8. The method for separating rhenium from an ammonium molybdate solution as claimed in claim 1, wherein in the step (4), the nanofiltration is performed intermittently, three times of concentrate recycling nanofiltration is performed, and the nanofiltration is stopped when the volume of the rhenium-rich liquid 2 is controlled to be 60-80% of the volume of the second concentrate.
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CN109179506B (en) * 2018-09-21 2021-01-01 中国地质科学院郑州矿产综合利用研究所 Method for synergistically recovering rhenium and molybdenum from molybdenum concentrate roasting leacheate
CN109321756A (en) * 2018-12-03 2019-02-12 中南大学 A kind of flue gas during smelting washs the device and method of high efficiente callback rhenium in waste acid
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