CN115572845A - Method for reducing content of molybdenum in N1923 loaded organic phase - Google Patents
Method for reducing content of molybdenum in N1923 loaded organic phase Download PDFInfo
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Abstract
A method for reducing the content of molybdenum in an N1923 loaded organic phase comprises the steps of firstly adjusting the pH of waste ammonia to be 8.5-9.6 by adopting an ammonia water adding mode, then using the waste ammonia water as a detergent to wash molybdenum in the N1923 loaded organic phase, leaving tungsten in the loaded organic phase as much as possible, and performing back extraction by using ammonium bicarbonate to obtain a molybdenum/tungsten ratio of more than 7:1, the strip liquor enters a tungsten-molybdenum evaporation crystallization link, the blank organic phase after strip is regenerated by sulfuric acid, and the blank organic phase returns to an extraction link again after reaching a regeneration standard, so that the purposes of eluting most of molybdenum in the organic phase and avoiding excessive loss of tungsten in the organic phase are achieved.
Description
The technical field is as follows:
the invention belongs to the field of tungsten-molybdenum separation in mineral separation, and particularly relates to a method for reducing the content of molybdenum in an N1923 loaded organic phase.
The background art comprises the following steps:
tungsten and molybdenum as non-renewable rare and precious metals are important strategic reserve resources in China, belong to the VIB group in common, are very similar in physicochemical properties due to the influence of the contraction effect of lanthanide series, and are often associated with each other in minerals. At present, the most effective method for separating and purifying tungsten and molybdenum is a solvent extraction method. The solvent extraction method has the advantages of high metal recovery rate, strong processing capacity, easy realization of automatic operation and the like, and is widely applied to industry.
Solvent extraction, one of the key steps in a hydrometallurgical process, is a unit operation that mainly utilizes the different solubilities of the components in the system in the solvent to separate the mixture. N1923 in an N1923+ isooctanol + sulfonated kerosene system is used as an extracting agent, isooctanol is used as a phase regulator, sulfonated kerosene is used as a diluent, and the proper organic phase composition is controlled to perform multi-stage countercurrent extraction with feed liquid containing tungsten and molybdenum, so that an N1923 loaded organic phase is obtained.
In the extraction process of the N1923+ isooctanol + sulfonated kerosene system, the problems of tungsten-molybdenum co-extraction and organic phase entrainment pollution exist, extracted tungsten-molybdenum enters a loaded organic phase and enters a strip liquor through strip agent strip, if the content of molybdenum in the organic phase is too high, a large amount of molybdenum enters an evaporation crystallization tungsten-molybdenum separation link, and difficulty is brought to the separation efficiency of the crystallized tungsten-molybdenum. Namely, the low tungsten-molybdenum ratio in the loaded organic phase is a key factor for restricting the evaporation crystallization separation efficiency of tungsten and molybdenum in the strip liquor, so that the improvement of the tungsten-molybdenum ratio in the loaded organic phase is particularly important. Due to the fact that in the existing workshop N1923+ isooctanol + sulfonated kerosene system, the mass concentration of molybdenum in the extracted loaded organic phase is too high, the tungsten-molybdenum ratio is reduced, and crystallization capacity is severely restricted. Therefore, in order to obtain a pure tungsten product, it is desirable to remove as much molybdenum as possible from the N1923 loaded organic phase.
The invention content is as follows:
in order to overcome the defects, the invention provides a method for reducing the content of molybdenum in an N1923 loaded organic phase.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a method for reducing the content of molybdenum in N1923 loaded organic phase comprises the following steps:
a. extraction: carrying out saturated extraction on an organic phase of a mixed system of N1923, isooctyl alcohol and sulfonated kerosene and a feed liquid containing tungsten and molybdenum to obtain an N1923 loaded organic phase;
b. preparing ammonia water: adding ammonia water into waste ammonia water obtained by passing the ammonium paratungstate waste liquid through a double-effect evaporation concentrator, and controlling the pH value to be 8.5-9.6;
c. and (3) countercurrent washing of molybdenum: washing the N1923 loaded organic phase in the step a with the ammonia water prepared in the step b, wherein the number of stages of countercurrent washing is 2-4, and the washing water-oil ratio is 2:1-5:1, washing reaction temperature is 25-45 ℃, washing reaction time is 20-40min, and standing phase separation time is 10-20min after washing;
d. and (3) countercurrent stripping of tungsten and molybdenum: and c, carrying out countercurrent back extraction on the washed loaded organic phase in the step c, wherein the number of the back extraction stages is 3-5, and controlling the tungsten-molybdenum ratio of the back extraction liquid end point to be more than 7:1, obtaining a back extraction solution and a blank organic phase;
e. and (3) evaporation and crystallization: obtaining a pure tungsten product from the strip liquor in an evaporation crystallization mode;
f. and (3) countercurrent regeneration: and d, carrying out countercurrent regeneration on the blank organic phase obtained in the step d, and returning the regenerated blank organic phase to the extraction link again.
In the N1923+ isooctanol + sulfonated kerosene system, the content of an organic phase component N1923: isooctyl alcohol: sulfonated kerosene is 1:2:7.
the content of tungsten in the N1923 loaded organic phase is higher than 55g/L, the content of molybdenum is higher than 20g/L, and the tungsten-molybdenum ratio is =1.5:1-2.5:1.
the ammonia concentration of the waste ammonia water is about 0.5-1.5g/L, the sodium content is lower than 0.005g/L, and the potassium content is lower than 0.01g/L.
The stripping agent is ammonium bicarbonate, the concentration of the stripping agent is 2.7-3.3mol/L, and the ratio of the ammonium bicarbonate to the ammonium bicarbonate is 1:1-3:1, the reaction time is 5-15min.
The control level of the blank organic phase for countercurrent regeneration is 2-4, the used regenerant is sulfuric acid, the concentration of the sulfuric acid is 1.5-2.5mol/L, and the pH value at the end of regeneration is controlled to be 2.0-3.0.
Due to the adoption of the technical scheme, the invention has the following advantages:
according to the method for reducing the content of molybdenum in the N1923 loaded organic phase, the waste ammonia water generated in workshop production is used as a detergent, so that the problems that the traditional waste ammonia water is large in generation amount, increases energy consumption and cannot be used are solved, and the source reduction of liquid waste is realized; meanwhile, reaction conditions required by washing are simple and effective, production equipment is simple, investment cost is low, efficient elution of molybdenum can be realized, and tungsten is guaranteed to be remained in an organic phase as much as possible.
Description of the drawings:
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a graph showing the effect of different pH values on the metal elution rate during counter current washing of molybdenum;
FIG. 3 is a schematic representation of the effect of different reaction temperatures on metal elution rates during counter current washing of molybdenum;
FIG. 4 is a graphical representation of the effect of different reaction times on metal elution rates during counter current washing of molybdenum;
FIG. 5 is a graph showing the effect of different water-oil ratios on metal elution rates during counter-current molybdenum scrubbing.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention is explained in more detail below with reference to fig. 1 and examples.
The first embodiment is as follows:
in this embodiment, the high-molybdenum N1923 loaded organic phase and the waste ammonia water come from a tungsten-molybdenum smelting plant, and are sampled and assayed, and in an N1923+ isooctanol + sulfonated kerosene system, the organic phase component N1923 is controlled: isooctyl alcohol: sulfonated kerosene is 1:2:7;
and (3) testing results: the concentration of tungsten in the N1923 loaded organic phase is 57.09g/L, the concentration of molybdenum in the loaded organic phase is 24.76g/L, the concentration of ammonia in the waste ammonia water is 0.75g/L, the content of sodium is 0.003g/L, the content of potassium is 0.008g/L, and the tungsten-molybdenum ratio is =2.3:1.
b. preparing ammonia water: adding ammonia water into waste ammonia water obtained by passing the ammonium paratungstate waste liquid through a double-effect evaporation concentrator to adjust the pH value, and controlling the pH value of the waste ammonia water to be 8.5;
c. and (3) counter-current washing of molybdenum: and c, washing the molybdenum by using the ammonia water obtained in the step b and an N1923 loaded organic phase, wherein the stage number of the counter-current washing is controlled to be 2, and the washing water-oil ratio is 2:1, washing reaction temperature is 25 ℃, washing reaction time is 20min, standing phase splitting time is 10min after washing, tungsten concentration in washed loaded organic phase is 53.21g/L, molybdenum concentration is 4.76g/L, molybdenum elution rate reaches 80.78%, and the main flow of tungsten-molybdenum back extraction is entered;
d. and (3) countercurrent stripping of tungsten and molybdenum: and c, loading the washed loaded organic phase obtained in the step c, performing countercurrent back extraction, wherein the number of back extraction stages is 3, the concentration of ammonium bicarbonate is controlled to be 2.7mol/L by a back extractant, and the ratio is 1:1, reaction time is 5min, and the tungsten-molybdenum ratio of the back extraction solution end point is controlled to be more than 7:1, enabling a blank organic phase after back extraction to enter an organic phase regeneration link;
e. evaporation and crystallization: the concentration of tungsten in the strip liquor is 116.60g/L, and the concentration of molybdenum in the strip liquor is 13.72g/L, and the strip liquor enters a tungsten-molybdenum evaporation crystallization link;
f. and (3) countercurrent regeneration: and d, carrying out countercurrent regeneration on the blank organic phase obtained in the step d, wherein the control level is 2 levels, the regenerant is sulfuric acid, the concentration is 1.5mol/L, the pH at the end of regeneration is controlled to be 2.0, and the blank organic phase returns to the extraction link again after regeneration.
Example two:
in this embodiment, the high-molybdenum N1923 loaded organic phase and the waste ammonia water come from a tungsten-molybdenum smelting plant, and are sampled and tested, and in an N1923+ isooctanol + sulfonated kerosene system, the organic phase component N1923: isooctyl alcohol: sulfonated kerosene is 1:2:7;
and (3) testing results: the tungsten concentration in the N1923 loaded organic phase is 52.11g/L, the molybdenum concentration is 29.09g/L, the ammonia concentration in the waste ammonia water is 1.02g/L, the sodium content is 0.004g/L, the potassium content is 0.009g/L, the tungsten-molybdenum ratio is =1.8:1.
b. preparing ammonia water: adding ammonia water into waste ammonia water obtained by passing the ammonium paratungstate waste liquid through a double-effect evaporation concentrator to adjust the pH value, and controlling the pH value of the waste ammonia water to be 9;
c. and (3) countercurrent washing of molybdenum: and c, washing molybdenum by using the ammonia water obtained in the step b and an N1923 loaded organic phase, wherein the stage number of counter-current washing is controlled to be 3, and the washing water-oil ratio is 4:1, washing at 35 ℃ for 30min, standing for 15min after washing, wherein the concentration of tungsten in the washed loaded organic phase is 49.84g/L, the concentration of molybdenum is 4.13g/L, the elution rate of molybdenum reaches 85.8 percent, and the loaded organic phase enters a main tungsten-molybdenum back extraction process;
d. and (3) countercurrent stripping of tungsten and molybdenum: and c, loading the washed loaded organic phase obtained in the step c, and performing countercurrent back extraction, wherein the number of back extraction stages is 4, the concentration of ammonium bicarbonate is controlled to be 3mol/L by a back extraction agent, and the ratio of the ammonium bicarbonate to the ammonium bicarbonate is 2:1, reaction time is 10min, and the tungsten-molybdenum ratio of the back extraction solution end point is controlled to be more than 7:1, feeding the blank organic phase subjected to back extraction into an organic phase regeneration link;
e. and (3) evaporation and crystallization: the concentration of tungsten in the strip liquor is 123.71g/L, and the concentration of molybdenum in the strip liquor is 11.45g/L, and the strip liquor enters a tungsten-molybdenum evaporation crystallization link;
f. and (3) countercurrent regeneration: and d, carrying out countercurrent regeneration on the blank organic phase obtained in the step d, wherein the control level is 3 levels, the regenerant is sulfuric acid, the concentration is 2mol/L, the pH at the end of regeneration is controlled to be 2.5, and the blank organic phase returns to the extraction link again after regeneration.
Example three:
in this embodiment, the high-molybdenum N1923 loaded organic phase and the waste ammonia water come from a tungsten-molybdenum smelting plant, and are sampled and tested, and in an N1923+ isooctanol + sulfonated kerosene system, the organic phase component N1923: isooctyl alcohol: sulfonated kerosene is 1:2:7;
and (3) testing results: the concentration of tungsten in the N1923 loaded organic phase is 60.11g/L, the concentration of molybdenum is 31.23g/L, the concentration of ammonia in the waste ammonia water is 1.48g/L, the content of sodium is 0.002g/L, the content of potassium is 0.007g/L, and the ratio of tungsten to molybdenum is =1.9:1.
b. preparing ammonia water: adding ammonia water into waste ammonia water obtained by passing the ammonium paratungstate waste liquid through a double-effect evaporation concentrator to adjust the pH value, and controlling the pH value of the waste ammonia water to be 9.6;
c. and (3) countercurrent washing of molybdenum: and c, washing molybdenum by using the ammonia water obtained in the step b and an N1923 loaded organic phase, wherein the stage number of counter-current washing is controlled to be 4, and the washing water-oil ratio is 5:1, washing at 45 ℃ for 40min, standing for 20min after washing, wherein the concentration of tungsten in the washed loaded organic phase is 58.74g/L, the concentration of molybdenum is 4.37g/L, the elution rate of molybdenum reaches 86%, and the main flow of tungsten-molybdenum back extraction is entered;
d. and (3) countercurrent stripping of tungsten and molybdenum: and c, loading the washed loaded organic phase obtained in the step c, performing countercurrent back extraction, wherein the number of back extraction stages is 5, the concentration of ammonium bicarbonate is controlled to be 3.3mol/L by a back extractant, and the ratio is 3:1, reaction time is 5min, and the tungsten-molybdenum ratio of the strip liquor terminal is controlled to be more than 7:1, feeding the blank organic phase subjected to back extraction into an organic phase regeneration link;
e. evaporation and crystallization: the concentration of tungsten in the strip liquor is 126.09g/L, and the concentration of molybdenum in the strip liquor is 12.18g/L, and the strip liquor enters a tungsten-molybdenum evaporation crystallization link;
f. and (3) countercurrent regeneration: and d, carrying out countercurrent regeneration on the blank organic phase obtained in the step d, wherein the control level is 4, the regenerant is sulfuric acid, the concentration is 2.5mol/L, the pH at the end of regeneration is controlled to be 3.0, and the blank organic phase returns to the extraction link again after regeneration.
As can be seen from the attached FIG. 2, when the molybdenum is washed in a countercurrent manner, the elution rate of tungsten and molybdenum is gradually increased along with the increase of the pH value, and when the pH value is more than 8.5, the elution rate of molybdenum is obviously increased, so that in order to allow the molybdenum to elute as much as possible, the pH value is in the range of 8.5-9.6 under the condition of no change of other conditions.
As can be seen from the attached FIG. 3, when the molybdenum is washed in a countercurrent manner, the temperature is between 25 ℃ and 50 ℃, the elution rates of tungsten and molybdenum are gradually reduced along with the increase of the temperature, but the influence of the temperature change on the elution rate of tungsten is small, the elution rate of molybdenum is large when the temperature is between 25 ℃ and 30 ℃, but the elution rate of molybdenum is reduced rapidly when the temperature reaches above 45 ℃, so that the reaction temperature is in the range of 25 ℃ to 45 ℃ under the condition that other conditions are not changed in order to elute the molybdenum as much as possible.
As can be seen from the attached FIG. 4, when the molybdenum is washed by countercurrent, the reaction time is within 20min, the elution rate of tungsten does not change obviously, although the elution rate of molybdenum increases gradually, the elution rate of molybdenum does not exceed 40%, when the time is within 20-40min, the elution rate of molybdenum increases obviously, and when the time exceeds 40min, the elution rates of tungsten and molybdenum are basically unchanged, so the optimal reaction time is 20-40min.
As can be seen from FIG. 5, in the countercurrent washing of molybdenum, the elution rate of tungsten and molybdenum gradually increases with the gradual increase of the water-oil ratio; when the water-oil ratio is 1; when the water-oil ratio is 2; when the water-oil ratio is 5.
The details of the above-mentioned parts are not described in detail since they are prior art.
Claims (6)
1. A method for reducing the content of molybdenum in N1923 loaded organic phase is characterized in that: the method comprises the following steps:
a. extraction: carrying out saturated extraction on an organic phase of a mixed system of N1923+ isooctyl alcohol + sulfonated kerosene and a feed liquid containing tungsten and molybdenum to obtain an N1923 loaded organic phase;
b. preparing ammonia water: adding ammonia water into waste ammonia water obtained by passing the ammonium paratungstate waste liquid through a double-effect evaporation concentrator, and controlling the pH value to be 8.5-9.6;
c. and (3) counter-current washing of molybdenum: washing the N1923 loaded organic phase in the step a with the ammonia water prepared in the step b, wherein the number of stages of countercurrent washing is 2-4, and the washing water-oil ratio is 2:1-5:1, washing reaction temperature is 25-45 ℃, washing reaction time is 20-40min, and standing phase separation time is 10-20min after washing;
d. and (3) countercurrent stripping of tungsten and molybdenum: and c, carrying out countercurrent back extraction on the washed loaded organic phase in the step c, wherein the number of the back extraction stages is 3-5, and controlling the tungsten-molybdenum ratio of the back extraction liquid end point to be more than 7:1, obtaining a back extraction solution and a blank organic phase;
e. and (3) evaporation and crystallization: obtaining a pure tungsten product from the strip liquor in an evaporation crystallization mode;
f. and (3) countercurrent regeneration: and d, carrying out countercurrent regeneration on the blank organic phase obtained in the step d, and returning the regenerated blank organic phase to the extraction link again.
2. The method for reducing the content of molybdenum in an N1923-loaded organic phase according to claim 1, wherein the method comprises the following steps: in the N1923+ isooctanol + sulfonated kerosene system, the content of an organic phase component N1923: isooctyl alcohol: sulfonated kerosene is 1:2:7.
3. the method for reducing the content of molybdenum in an N1923-loaded organic phase according to claim 1, wherein: the content of tungsten in the N1923 loaded organic phase is higher than 55g/L, the content of molybdenum is higher than 20g/L, and the tungsten-molybdenum ratio is =1.5:1-2.5:1.
4. the method for reducing the content of molybdenum in an N1923-loaded organic phase according to claim 1, wherein the method comprises the following steps: the ammonia concentration of the waste ammonia water is about 0.5-1.5g/L, the sodium content is lower than 0.005g/L, and the potassium content is lower than 0.01g/L.
5. The method for reducing the content of molybdenum in an N1923-loaded organic phase according to claim 1, wherein the method comprises the following steps: the stripping agent is ammonium bicarbonate, the concentration of the stripping agent is 2.7-3.3mol/L, and the ratio of the ammonium bicarbonate to the ammonium bicarbonate is 1:1-3:1, the reaction time is 5-15min.
6. The method for reducing the content of molybdenum in an N1923-loaded organic phase according to claim 1, wherein: the control level of the blank organic phase for countercurrent regeneration is 2-4, the used regenerant is sulfuric acid, the concentration of the sulfuric acid is 1.5-2.5mol/L, and the pH value at the end of regeneration is controlled to be 2.0-3.0.
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