CN110358920B - Method for separating vanadium from vanadium-chromium waste residue - Google Patents

Method for separating vanadium from vanadium-chromium waste residue Download PDF

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CN110358920B
CN110358920B CN201910699958.7A CN201910699958A CN110358920B CN 110358920 B CN110358920 B CN 110358920B CN 201910699958 A CN201910699958 A CN 201910699958A CN 110358920 B CN110358920 B CN 110358920B
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vanadium
chromium
waste residue
slurry
chromium waste
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CN110358920A (en
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张一敏
王露瑶
薛楠楠
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Wuhan University of Science and Engineering WUSE
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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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/005—Preliminary treatment of scrap
    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Organic Chemistry (AREA)
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  • Environmental & Geological Engineering (AREA)
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Abstract

The invention relates to a method for separating vanadium from vanadium-chromium waste residue. The technical scheme is as follows: mixing sodium sulfite and sodium bisulfite in the mass ratio of (1-4) to 1 to obtain the reducing agent. Mixing the vanadium-chromium waste residue powder with water according to the solid-liquid ratio of 1 to (1-2) Kg/L to obtain slurry. Adding the slurry into a closed reactor, adding a reducing agent into the closed reactor, and stirring for 30-60 min at the temperature of 20-40 ℃ and at the speed of 100-200 r/min to obtain a raw material slurry; the addition amount of the reducing agent is 3-9 wt% of the vanadium-chromium waste residue powder. Adding concentrated sulfuric acid into the reduced slurry according to the proportion of adding 0.02-0.040L of concentrated sulfuric acid into each kilogram of vanadium-chromium waste residue powder, and stirring for 1-4 hours at the temperature of 20-40 ℃ and under the condition of 200-400 r/min to obtain reacted slurry. And carrying out solid-liquid separation on the reacted slurry to obtain vanadium-rich solution and chromium-containing leaching residue. The method has the characteristics of high vanadium leaching rate, good vanadium-chromium separation effect and low energy consumption.

Description

Method for separating vanadium from vanadium-chromium waste residue
Technical Field
The invention belongs to the technical field of resource utilization of vanadium-chromium waste residues. In particular to a method for separating vanadium from vanadium-chromium waste residue.
Background
The vanadium-chromium waste slag is mainly from metallurgy, yellow phosphorus production and special steel smelting additive production enterprises, and is an important vanadium-containing secondary resource. The chemical composition and structure of the vanadium-chromium waste residue are greatly influenced by the waste residue generation process. Meanwhile, because the properties of vanadium and chromium are very similar, a large amount of chromium is easy to enter the leaching solution in the vanadium leaching process, an effective separation technology is lacked, and most enterprises can only adopt landfill treatment after detoxification.
At present, the vanadium extraction process from vanadium-chromium waste slag usually adopts a process of roasting by adding salt and leaching to extract vanadium. The patent technology of 'a method for separating and recovering vanadium and chromium from vanadium-chromium slag' (CN 104178637A) adopts calcification roasting-acid leaching to extract vanadium, and then sodium treatment roasting-water leaching is carried out on the acid leaching slag after vanadium extraction to extract chromium. The method can achieve the aim of recovering vanadium and chromium step by step. However, the two-stage salt adding roasting is adopted, the roasting temperature reaches 800 ℃, and the problems of long process flow, high energy consumption and the like exist. The patent technology of 'a method for preparing vanadium pentoxide by using high-chromium vanadium slag' (CN 109161677A) adopts (NH)4)2SO4—H2SO4Leaching vanadium slag by a synergistic system, and obtaining vanadium-containing leachate and chromium-containing leaching slag by solid-liquid separation. Although the leaching of chromium is avoided in the vanadium leaching process, the leaching processBefore the treatment, the vanadium-containing slag is treated by a calcification roasting process at a high temperature of 700-1000 ℃.
A process for extracting V and Cr from solid material containing V and Cr (CN 108315572A) includes such steps as mixing solid material containing V and Cr, reducing agent and acid liquid, direct reduction extracting reaction, and adding V to the mixture2O5Is reduced to V2O4And reacting with acid to finally obtain the vanadium-chromium-containing leaching solution. The reducing agent selected by the method is one of sulfur dioxide, sodium sulfite, sodium thiosulfate and sodium metabisulfite. Although the method can effectively extract vanadium and chromium in the materials, the vanadium and the chromium are leached synchronously, and the leaching process has no selectivity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a method for separating vanadium from vanadium-chromium waste residues, which has high vanadium leaching rate, good vanadium-chromium separation effect and low process energy consumption.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following specific steps:
step one, ore grinding and dissociation
And grinding the vanadium-chromium waste slag until the granularity is less than 74 mu m and accounts for 70-85 wt%, thereby obtaining vanadium-chromium waste slag powder.
Step two, reduction inhibition
Mixing sodium sulfite and sodium bisulfite according to the mass ratio of (1-4) to 1 to obtain the reducing agent.
Mixing the vanadium-chromium waste residue powder with water according to the solid-liquid ratio of 1 to (1-2) Kg/L to obtain slurry; and adding the slurry into a closed reactor, adding the reducing agent into the closed reactor, and stirring for 30-60 min at the temperature of 20-40 ℃ and at the speed of 100-200 r/min to obtain the reduced raw material slurry.
The addition amount of the reducing agent is 3-9 wt% of the vanadium-chromium waste residue powder.
Step three, acidifying and dissolving
Adding 0.02-0.040L of concentrated sulfuric acid into each kilogram of vanadium-chromium waste residue powder, adding the concentrated sulfuric acid into the reduced slurry, and stirring for 1-4 hours at the temperature of 20-40 ℃ and under the condition of 200-400 r/min to obtain slurry after reaction.
The concentration of the concentrated sulfuric acid is 80-98 vol%.
Step four, solid-liquid separation
And carrying out solid-liquid separation on the reacted slurry to obtain vanadium-rich solution and chromium-containing leaching residue.
The vanadium-chromium waste residue is obtained after the vanadium-titanium magnetite iron and steel smelting production process is processed by a complexation-decomplexation technology. Wherein: the total vanadium content is V2O510-20 wt% of vanadium, and the main existing form of vanadium is CaV2O6，CaV2O6The vanadium content accounts for 60-90 wt% of the total vanadium content; total chromium content in CrO3Calculated as 3-10 wt%, the main existing form of chromium is CrO3，CrO3The content of chromium is 50-95 wt% of the total content of chromium.
Compared with the prior art, the method has the following positive effects:
(1) the invention adopts the reducing agent to reduce the electrode potential of the reduced raw material slurry and inhibit Cr in the vanadium-chromium waste residue2O3The dissolution of (2) creates a reducing environment for the conversion of V (V) → V (IV), so that the vanadium and the chromium can be effectively separated. The leaching rate of chromium is lower than 2 percent through measurement.
(2) The invention adopts acidification dissolution to reduce the pH value of the raw material slurry, accelerates the reduction conversion of V (V) → V (IV), makes vanadium dissolve out more easily, and greatly improves the vanadium leaching rate. Through determination, the leaching rate of vanadium can reach 80-95%.
(3) According to the invention, through solid-liquid separation, the vanadium concentration in the obtained vanadium-rich liquid is more than 15g/L, and the chromium concentration is less than 0.2g/L, so that the vanadium-rich liquid can be directly used for a vanadium precipitation process, and the influence of chromium on the vanadium precipitation process is avoided.
(4) The reaction temperature required in the acidification and dissolution process is only 20-40 ℃, external heating is basically not required, and the energy consumption is low.
Therefore, the method has the characteristics of high vanadium leaching rate, good vanadium-chromium separation effect and low energy consumption.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
In this embodiment:
the vanadium-chromium waste residue is obtained after the vanadium-titanium magnetite iron and steel smelting production process is processed by a complexation-decomplexation technology.
Wherein: the total vanadium content is V2O510-20 wt% of vanadium, and the main existing form of vanadium is CaV2O6，CaV2O6The vanadium content accounts for 60-90 wt% of the total vanadium content; total chromium content in CrO3Calculated as 3-10 wt%, the main existing form of chromium is CrO3，CrO3The content of chromium is 50-95 wt% of the total content of chromium.
The detailed description is omitted in the embodiments.
Example 1
A method for separating vanadium from vanadium-chromium waste residue. The method of the embodiment comprises the following steps:
step one, ore grinding and dissociation
And grinding the vanadium-chromium waste slag until the granularity is less than 74 mu m and accounts for 70-85 wt%, thereby obtaining vanadium-chromium waste slag powder.
Step two, reduction inhibition
Mixing sodium sulfite and sodium bisulfite according to the mass ratio of (1-2) to 1 to obtain the reducing agent.
Mixing the vanadium-chromium waste residue powder with water according to the solid-liquid ratio of 1 to (1-2) Kg/L to obtain slurry; and adding the slurry into a closed reactor, adding the reducing agent into the closed reactor, and stirring for 30-40 min at the temperature of 20-40 ℃ and at the speed of 100-200 r/min to obtain the reduced raw material slurry.
The addition amount of the reducing agent is 6-9 wt% of the vanadium-chromium waste residue powder.
Step three, acidifying and dissolving
Adding 0.02-0.028L of concentrated sulfuric acid into each kilogram of vanadium-chromium waste residue powder, adding the concentrated sulfuric acid into the reduction slurry, and stirring for 1-2 hours at the temperature of 20-30 ℃ and under the condition of 200-300 r/min to obtain slurry after reaction.
The concentration of the concentrated sulfuric acid is 80-98 vol%.
Step four, solid-liquid separation
And carrying out solid-liquid separation on the reacted slurry to obtain vanadium-rich solution and chromium-containing leaching residue.
In this embodiment: the leaching rate of vanadium is 80-88%; the leaching rate of chromium is 1.5-2%.
Example 2
A method for separating vanadium from vanadium-chromium waste residue. The method of the embodiment comprises the following steps:
step one, ore grinding and dissociation
And grinding the vanadium-chromium waste slag until the granularity is less than 74 mu m and accounts for 70-85 wt%, thereby obtaining vanadium-chromium waste slag powder.
Step two, reduction inhibition
Mixing sodium sulfite and sodium bisulfite according to the mass ratio of sodium sulfite to sodium bisulfite of (2-3) to 1 to obtain the reducing agent.
Mixing the vanadium-chromium waste residue powder with water according to the solid-liquid ratio of 1 to (1-2) Kg/L to obtain slurry; and adding the slurry into a closed reactor, adding the reducing agent into the closed reactor, and stirring for 40-50 min at the temperature of 20-40 ℃ and at the speed of 100-200 r/min to obtain the reduced raw material slurry.
The addition amount of the reducing agent is 5-7 wt% of the vanadium-chromium waste residue powder.
Step three, acidifying and dissolving
Adding 0.025-0.035L of concentrated sulfuric acid into each kilogram of vanadium-chromium waste residue powder, adding the concentrated sulfuric acid into the reduction slurry, and stirring for 2-3 h at the temperature of 25-35 ℃ and at the speed of 250-350 r/min to obtain slurry after reaction.
The concentration of the concentrated sulfuric acid is 80-98 vol%.
Step four, solid-liquid separation
And carrying out solid-liquid separation on the reacted slurry to obtain vanadium-rich solution and chromium-containing leaching residue.
In this embodiment: the leaching rate of vanadium is 85-92%; the leaching rate of chromium is 1-1.5%.
Example 3
A method for separating vanadium from vanadium-chromium waste residue. The method of the embodiment comprises the following steps:
step one, ore grinding and dissociation
And grinding the vanadium-chromium waste slag until the granularity is less than 74 mu m and accounts for 70-85 wt%, thereby obtaining vanadium-chromium waste slag powder.
Step two, reduction inhibition
Mixing sodium sulfite and sodium bisulfite according to the mass ratio of sodium sulfite to sodium bisulfite of (3-4) to 1 to obtain the reducing agent.
Mixing the vanadium-chromium waste residue powder with water according to the solid-liquid ratio of 1 to (1-2) Kg/L to obtain slurry; and adding the slurry into a closed reactor, adding the reducing agent into the closed reactor, and stirring for 50-60 min at the temperature of 20-40 ℃ and at the speed of 100-200 r/min to obtain the reduced raw material slurry.
The addition amount of the reducing agent is 3-6 wt% of the vanadium-chromium waste residue powder.
Step three, acidifying and dissolving
Adding 0.03-0.040L of concentrated sulfuric acid into each kilogram of vanadium-chromium waste residue powder, adding the concentrated sulfuric acid into the reduced slurry, and stirring for 3-4 hours at the temperature of 30-40 ℃ and under the condition of 300-400 r/min to obtain slurry after reaction.
The concentration of the concentrated sulfuric acid is 80-98 vol%.
Step four, solid-liquid separation
And carrying out solid-liquid separation on the reacted slurry to obtain vanadium-rich solution and chromium-containing leaching residue.
In this embodiment: the leaching rate of vanadium is 90-95%; the leaching rate of chromium is lower than 1 percent.
Compared with the prior art, the specific implementation mode has the following positive effects:
(1) the specific embodiment adopts the reducing agent to reduce the electrode potential of the reduced raw material slurry and inhibit Cr in the vanadium-chromium waste residue2O3The dissolution of (2) creates a reducing environment for the conversion of V (V) → V (IV), so that the vanadium and the chromium can be effectively separated. The leaching rate of chromium is lower than 2 percent through measurement.
(2) The specific embodiment adopts acidification dissolution to reduce the pH value of the raw material slurry, accelerates the reduction conversion of V (V) → V (IV), makes vanadium dissolve out more easily, and greatly improves the vanadium leaching rate. Through determination, the leaching rate of vanadium can reach 80-95%.
(3) According to the specific embodiment, the vanadium concentration in the vanadium-rich liquid obtained through solid-liquid separation is more than 15g/L, and the chromium concentration is less than 0.2g/L, so that the vanadium-rich liquid can be directly used for a vanadium precipitation process, and the influence of chromium on the vanadium precipitation process is avoided.
(4) The reaction temperature required in the acidification and dissolution process of the specific embodiment is only 20-40 ℃, external heating is basically not required, and the energy consumption is low.
Therefore, the specific embodiment has the characteristics of high vanadium leaching rate, good vanadium-chromium separation effect and low energy consumption.

Claims (1)

1. A method for separating vanadium from vanadium-chromium waste residue is characterized by comprising the following specific steps:
step one, ore grinding and dissociation
Grinding the vanadium-chromium waste residue until the particle size is less than 74 mu m and accounts for 70-85 wt%, so as to obtain vanadium-chromium waste residue powder;
step two, reduction inhibition
Mixing sodium sulfite and sodium bisulfite according to the mass ratio of the sodium sulfite to the sodium bisulfite of (1-4) to 1 to obtain a reducing agent;
mixing the vanadium-chromium waste residue powder with water according to the solid-liquid ratio of 1 to (1-2) Kg/L to obtain slurry; adding the slurry into a closed reactor, adding the reducing agent into the closed reactor, and stirring for 30-60 min at the temperature of 20-40 ℃ and at the speed of 100-200 r/min to obtain a returned raw material slurry;
the addition amount of the reducing agent is 3-9 wt% of the vanadium-chromium waste residue powder;
step three, acidifying and dissolving
Adding 0.02-0.040L of concentrated sulfuric acid into each kilogram of vanadium-chromium waste residue powder, adding the concentrated sulfuric acid into the reduced slurry, and stirring for 1-4 hours at the temperature of 20-40 ℃ and under the condition of 200-400 r/min to obtain reacted slurry;
the concentration of the concentrated sulfuric acid is 80-98 vol%;
step four, solid-liquid separation
Carrying out solid-liquid separation on the reacted slurry to obtain vanadium-rich solution and chromium-containing leaching residue;
the vanadium-chromium waste residue is obtained after the vanadium-titanium magnetite iron and steel smelting production process is processed by a complexation-decomplexation technology;
wherein: the total vanadium content is V2O510-20 wt% of vanadium, and the main existing form of vanadium is CaV2O6，CaV2O6The vanadium content accounts for 60-90 wt% of the total vanadium content; total chromium content in CrO3Calculated as 3-10 wt%, the main existing form of chromium is CrO3，CrO3The content of chromium is 50-95 wt% of the total content of chromium.
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CN112225381B (en) * 2020-07-09 2022-04-26 桂林理工大学 Treatment method of chromium-containing wastewater
CN111876615B (en) * 2020-07-10 2022-07-05 武汉科技大学 Method for separating vanadium and molybdenum from high-chromium waste residue
CN113416847B (en) * 2021-07-05 2022-05-31 昆明理工大学 Method for recycling, reducing and harmlessly treating vanadium extraction tailings
CN114231759A (en) * 2021-12-20 2022-03-25 攀枝花市阳润科技有限公司 Method for resource utilization of impurity-removed mud

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US4119696A (en) * 1977-11-14 1978-10-10 Uop Inc. Production of titanium metal values
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CN105695760A (en) * 2016-03-02 2016-06-22 东北大学 Method for carrying out two-stage countercurrent leaching on chromium-containing vanadium slag and extracting vanadium and chromium in separating manner
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US3679397A (en) * 1969-12-29 1972-07-25 Regents New Mexico Inst Of Min Bacterial leaching process
US4119696A (en) * 1977-11-14 1978-10-10 Uop Inc. Production of titanium metal values
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CN103966438A (en) * 2014-05-14 2014-08-06 攀钢集团攀枝花钢铁研究院有限公司 Method for electrolytic separation of vanadium and chromium in vanadium-chromium containing solution
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