CN100543158C - A kind of method for purifying and enriching of low-concentration vanadium-containing water solution - Google Patents

A kind of method for purifying and enriching of low-concentration vanadium-containing water solution Download PDF

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CN100543158C
CN100543158C CNB2008100473762A CN200810047376A CN100543158C CN 100543158 C CN100543158 C CN 100543158C CN B2008100473762 A CNB2008100473762 A CN B2008100473762A CN 200810047376 A CN200810047376 A CN 200810047376A CN 100543158 C CN100543158 C CN 100543158C
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vanadium
resin
concentration
low
containing water
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CN101260467A (en
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张一敏
刘涛
黄晶
陈铁军
康兴东
张华丽
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Wuhan University of Science and Engineering WUSE
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Wuhan University of Science and Engineering WUSE
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
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Abstract

The present invention is specifically related to a kind of method for purifying and enriching of low-concentration vanadium-containing water solution.Its scheme is earlier at V 2O 5Concentration is the scavenging agent that adds 0.6~10g/L in the low-concentration vanadium-containing water solution of 2000~5000mg/L, is adjusted to pH=6~8 behind the mixing; Again with this low-concentration vanadium-containing water solution with 2.0~10.0mLh -1ML -1The speed of wet resin is carried out ion-exchange absorption by strongly basic anion exchange resin, and is saturated as to contain the vanadium resin and adsorb liquid down to strongly basic anion exchange resin absorption; The mixing solutions of preparing 3~5wt%NaOH+8~13wt%NaCl then is as strippant, and the consumption of strippant is to contain 3~5 times of vanadium resin volume, and strippant is with 0.8~1.6mLh -1ML -1The speed of wet resin is carried out desorb by containing the vanadium resin, gets rich vanadium liquid; The last scavenging agent that adds 0.1~2.5g/L in rich vanadium liquid, solid-liquid separation gets scavenging solution.The present invention has the clarification time of saving and scavenging agent consumption, vanadium lose minimizing, good purification, technology characteristic of simple.

Description

A kind of method for purifying and enriching of low-concentration vanadium-containing water solution
Technical field
The invention belongs to the purification enrichment technical field that contains the vanadium aqueous solution.Relate in particular to a kind of method for purifying and enriching of low-concentration vanadium-containing water solution.
Background technology
It is relatively low that the overwhelming majority contains the vanadium grade of vanadium raw materials, the main both at home and abroad wet method process for extracting vanadium that adopts.Because various places contain the different of vanadium raw materials and integrated artistic requirement, water logging goes out at the wet method process for extracting vanadium and still occupies an important position.
Because to contain vanadium raw materials vanadium grade lower usually, to contain vanadium solution vanadium concentration also lower so leach gained, and foreign matter content such as other metal ions is higher in the solution, as if directly carrying out precipitation operation, gained V 2O 5Product purity have only 86% usually (" non-ferrous extractive metallurgy handbook editorial board. " and under the rare refractory metal of non-ferrous extractive metallurgy handbook, Beijing: metallurgical industry press, 1999:335), can not satisfy application requiring far away.Therefore, production high purity vanadium product must carry out purification enrichment to the low-concentration vanadium-containing infusion solution to be handled.
For a long time, the purification enrichment that contains vanadium solution both at home and abroad mainly contains extraction and ion-exchange dual mode.The extraction process operating speed is fast, easy and simple to handle, but the extraction process route is long, extraction conditions harshness, fluctuation of service.Comparatively speaking, ion exchange process (Liu Guoan, Li Liaosha, Yu Liang. contain useless admittedly vanadium extraction technology of vanadium and prospect. metal mine, 2003 (10): 63) selectivity is strong, raw materials consumption is few, environmental pollution is little, reusable edible.
During wet method vanadium extraction is both at home and abroad used at present, contain the employed ion exchange resin of vanadium infusion based on strongly basic anion exchange resin.Containing the vanadium aqueous solution can realize purification enrichment by using strongly basic anion exchange resin, but in operation process, contains also enrichments relatively of impurity such as Si, P in the vanadium aqueous solution, As, Mn, Al, influences the quality product of precipitation operation, causes precipitation rate instability.Removal of impurities (Xu Hongbo is precipitated to containing before the vanadium aqueous solution then adopts ion-exchange in domestic advanced minority enterprise and scientific research institutions, Luo Yunli, the leaves of pulse plants is good for Kui. vanadium leachate dephosphorization research, the Sichuan non-ferrous metal, 2002 (3): 29), but this mode medicament (being generally calcium chloride or calcium oxide) consumption is big, the vanadium loss is big, and produce a large amount of mud and can not handle on time, an operation is in time sent qualified liquid backward, the continuity that influence is produced.The follow-up precipitation of the rich vanadium liquid of gained is still unstable behind the purification and impurity removal, particularly for the water logging process for extracting vanadium that adopts partial material and water circulation comprehensive to utilize, because impurity is just more obvious to the unsettled influence of precipitation also by the enrichment that circulates simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of technology simple, save time, the method for purifying and enriching of the scavenging agent consumption is few, the rate of recovery of good purification, vanadium is high low-concentration vanadium-containing water solution.
To achieve these goals, the technical solution used in the present invention is: earlier at V 2O 5Concentration is the scavenging agent that adds 0.6~10g/L in the low-concentration vanadium-containing water solution of 2000~5000mg/L, is adjusted to pH=6~8 behind the mixing; Again with this low-concentration vanadium-containing water solution with 2.0~10.0mLh -1ML -1The speed of wet resin is carried out ion-exchange absorption by strongly basic anion exchange resin, and is saturated as to contain the vanadium resin and adsorb liquid down to strongly basic anion exchange resin absorption; The mixing solutions of preparing 3~5wt%NaOH+8~13wt%NaCl then is as strippant, and the consumption of strippant is to contain 3~5 times of vanadium resin volume, and strippant is with 0.8~1.6mLh -1ML -1The speed of wet resin is carried out desorb by containing the vanadium resin, gets rich vanadium liquid; The last scavenging agent that adds 0.1~2.5g/L in rich vanadium liquid, solid-liquid separation gets scavenging solution.
Wherein: described scavenging agent is a kind of in the calcium salt of solubility or the magnesium salts; Described strongly basic anion exchange resin is that model is 201 * 7,201 * 4, a kind of in the strongly basic anion exchange resin of D202, D231.
Owing to adopt technique scheme, the present invention adds a small amount of scavenging agent in low-concentration vanadium-containing water solution, saved the use of the preceding setting tank of common strongly basic anion exchange resin ion-exchange, saved 10~16h sedimentation time, the vanadium loss reduces more than 1%, desorption efficiency improves 3~5%, rich vanadium liquid through the ion-exchange gained directly adds the scavenging agent removal of impurities, simplify rich vanadium liquid and reconciled pH value back adding scavenging agent purification and impurity removal operation, the scavenging agent consumption is saved more than 83%, reached the purification and impurity removal effect, for realizing containing ammonium salt precipitation production high purity V behind the vanadium aqueous solution purification enrichment 2O 5(grade is greater than 99%) and whole wet method vanadium extraction total yield improve lays a good foundation.
Therefore, the present invention has and saves clarification time and scavenging agent consumption, vanadium loss minimizing, good purification, technology characteristic of simple.
Description of drawings
Fig. 1 is a kind of process flow sheet of the present invention.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments:
Embodiment 1:
A kind of method for purifying and enriching of low-concentration vanadium-containing water solution, its method for purifying and enriching be as shown in Figure 1: earlier at V 2O 5Concentration is the CaCl that adds 0.6~5.8g/L in the low-concentration vanadium-containing water solution of 2000~3500mg/L 2, be adjusted to pH=6~8 behind the mixing; Again with this low-concentration vanadium-containing water solution with 2.0~3.7mLh -1ML -1The speed of wet resin is that 201 * 7 strongly basic anion exchange resin carries out ion-exchange absorption by model, is that 201 * 7 strongly basic anion exchange resin absorption is saturated as to contain vanadium resin and absorption liquid down to model; The mixing solutions of preparing 3~4wt%NaOH+8~11wt%NaCl then is as strippant, and the consumption of strippant is to contain 3~4 times of vanadium resin volume, and strippant is with 0.8~1.1mLh -1ML -1The speed of wet resin is carried out desorb by containing the vanadium resin, gets rich vanadium liquid; The last CaCl that in rich vanadium liquid, adds 0.1~1.2g/L 2, solid-liquid separation gets scavenging solution.Scavenging solution enters follow-up ammonium salt precipitation technology.
Embodiment 2:
A kind of method for purifying and enriching of low-concentration vanadium-containing water solution, its method for purifying and enriching be as shown in Figure 1: earlier at V 2O 5Concentration is the Ca (NO that adds 5.8~10g/L in the low-concentration vanadium-containing water solution of 3500~5000mg/L 3) 2, be adjusted to pH=6~8 behind the mixing; Again with this low-concentration vanadium-containing water solution with 5.1~7.9mLh -1ML -1The speed of wet resin is that 201 * 4 strongly basic anion exchange resin carries out ion-exchange absorption by model, is that 201 * 4 strongly basic anion exchange resin absorption is saturated as to contain vanadium resin and absorption liquid down to model; The mixing solutions of preparing 4~5wt%NaOH+11~13wt%NaCl then is as strippant, and the consumption of strippant is to contain 4~5 times of vanadium resin volume, and strippant is with 1.3~1.4mLh -1ML -1The speed of wet resin is carried out desorb by containing the vanadium resin, gets rich vanadium liquid; Last Ca (the NO that in rich vanadium liquid, adds 1.2~2.5g/L 3) 2, solid-liquid separation gets scavenging solution.Scavenging solution enters follow-up ammonium salt precipitation technology.
Embodiment 3:
A kind of method for purifying and enriching of low-concentration vanadium-containing water solution, its method for purifying and enriching be as shown in Figure 1: earlier at V 2O 5Concentration is the MgCl that adds 0.6~4.6g/L in the low-concentration vanadium-containing water solution of 2000~3000mg/L 2, be adjusted to pH=6~8 behind the mixing; Again with this low-concentration vanadium-containing water solution with 3.7~5.1mLh -1ML -1The speed of wet resin is that the strongly basic anion exchange resin of D202 carries out ion-exchange absorption by model, is that the strongly basic anion exchange resin absorption of D202 is saturated as to contain vanadium resin and absorption liquid down to model; The mixing solutions of preparing 3~4wt%NaOH+8~11wt%NaCl then is as strippant, and the consumption of strippant is to contain 3~4 times of vanadium resin volume, and strippant is with 1.1~1.3mLh -1ML -1The speed of wet resin is carried out desorb by containing the vanadium resin, gets rich vanadium liquid; The last MgCl that in rich vanadium liquid, adds 0.1~1.5g/L 2, solid-liquid separation gets scavenging solution.Scavenging solution enters follow-up ammonium salt precipitation technology.
Embodiment 4:
Earlier at V 2O 5Concentration is the Mg (NO that adds 4.6~10g/L in the low-concentration vanadium-containing water solution of 3000~5000mg/L 3) 2, be adjusted to pH=6~8 behind the mixing; Again with this low-concentration vanadium-containing water solution with 7.9~10mLh -1ML -1The speed of wet resin is that the strongly basic anion exchange resin of D231 carries out ion-exchange absorption by model, is that the strongly basic anion exchange resin absorption of D231 is saturated as to contain vanadium resin and absorption liquid down to model; The mixing solutions of preparing 4~5wt%NaOH+11~13wt%NaCl then is as strippant, and the consumption of strippant is to contain 4~5 times of vanadium resin volume, and strippant is with 1.4~1.6mLh -1ML -1The speed of wet resin is carried out desorb by containing the vanadium resin, gets rich vanadium liquid; Last Mg (the NO that in rich vanadium liquid, adds 1.5~2.5g/L 3) 2, solid-liquid separation gets scavenging solution.Scavenging solution enters follow-up ammonium salt precipitation technology.
Present embodiment 1~4 all adds a small amount of scavenging agent in low-concentration vanadium-containing water solution, saved the use of the preceding setting tank of common strongly basic anion exchange resin ion-exchange, saved 12~16h sedimentation time, the vanadium rate of loss is only below 1.54%, ion-exchange desorb rate is more than 98.56%, through the rich vanadium liquid of ion-exchange gained, directly add the scavenging agent removal of impurities, simplify rich vanadium liquid and reconciled pH value back adding scavenging agent purification and impurity removal operation, the scavenging agent consumption is saved more than 85%, reached the purification and impurity removal effect, for realizing containing ammonium salt precipitation production high purity V behind the vanadium aqueous solution purification enrichment 2O 5(grade is greater than 99%) and whole wet method vanadium extraction total yield improve lays a good foundation.
Therefore, this embodiment has and saves clarification time and scavenging agent consumption, vanadium loss minimizing, good purification, technology characteristic of simple.

Claims (2)

1, a kind of method for purifying and enriching of low-concentration vanadium-containing water solution is characterized in that earlier at V 2O 5Concentration is the scavenging agent that adds 0.6~10g/L in the low-concentration vanadium-containing water solution of 2000~5000mg/L, is adjusted to pH=6~8 behind the mixing; Again with this low-concentration vanadium-containing water solution with 2.0~10.0mLh -1ML -1The speed of wet resin is carried out ion-exchange absorption by strongly basic anion exchange resin, and is saturated as to contain the vanadium resin and adsorb liquid down to strongly basic anion exchange resin absorption; The mixing solutions of preparing 3~5wt%NaOH+8~13wt%NaCl then is as strippant, and the consumption of strippant is to contain 3~5 times of vanadium resin volume, and strippant is with 0.8~1.6mLh -1ML -1The speed of wet resin is carried out desorb by containing the vanadium resin, gets rich vanadium liquid; The last scavenging agent that in rich vanadium liquid, adds 0.1~2.5g/L, solid-liquid separation gets scavenging solution;
Described scavenging agent is a kind of in the calcium salt of solubility or the magnesium salts.
2, method for purifying and enriching according to claim 1 is characterized in that described strongly basic anion exchange resin is that model is 201 * 7,201 * 4, a kind of in the strongly basic anion exchange resin of D202, D231.
CNB2008100473762A 2008-04-17 2008-04-17 A kind of method for purifying and enriching of low-concentration vanadium-containing water solution Expired - Fee Related CN100543158C (en)

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CN102864318B (en) * 2012-10-16 2014-04-16 长沙矿冶研究院有限责任公司 Method for recycling vanadium from acid vanadium-containing solution containing silicon and phosphorus
CN103572062A (en) * 2013-10-17 2014-02-12 攀钢集团攀枝花钢铁研究院有限公司 Method for recovering vanadium from desilication slag
CN104294045B (en) * 2014-11-05 2016-10-05 中南大学 Method containing Vanadotungstic acid. saline solution deeply removing vanadium
CN105149017B (en) * 2015-10-08 2018-09-21 武汉科技大学 A kind of ion-exchange process containing vanadium solution
CN108502928B (en) * 2017-02-23 2020-10-27 中国科学院过程工程研究所 Production method for deep vanadium removal in chromite calcium-free roasting process
CN108913889A (en) * 2018-06-20 2018-11-30 中国地质大学(北京) A kind of method of Microorganism Leaching vanadium and selective enrichment vanadium
CN109607612A (en) * 2018-12-24 2019-04-12 孙昕 Vanadium in a kind of discarded SCR denitration, tungsten, titanium resource recycling method

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