CN104294033A - Vanadium extracting process for silicate type vanadium ore - Google Patents

Vanadium extracting process for silicate type vanadium ore Download PDF

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Publication number
CN104294033A
CN104294033A CN201310299567.9A CN201310299567A CN104294033A CN 104294033 A CN104294033 A CN 104294033A CN 201310299567 A CN201310299567 A CN 201310299567A CN 104294033 A CN104294033 A CN 104294033A
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vanadium
roasting
resin
temperature
section
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张明
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Wuxi Huaye Iron & Steel Co Ltd
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Wuxi Huaye Iron & Steel 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
    • 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
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a vanadium extracting process for a silicate type vanadium ore. The process adopts a roasting leaching process of first-stage roasting, second-stage additive roasting and acid leaching according to the characteristics of the silicate type vanadium ore, so that the leaching effect is good, and the leaching rate of vanadium is higher than 85%.

Description

A kind of silicate-type navajoite process for extracting vanadium
Technical field
The present invention relates to vanadium extraction field, be specifically related to a kind of silicate-type navajoite process for extracting vanadium.
Background technology
Extract the difference of raw material due to kind, character and content of vanadium, treatment process is different.At present, the main raw material of vanadium extraction has navajoite, bone coal, slag, spent vanadium catalyst and contains vanadium material etc., and its process for extracting vanadium generally all will through hydrometallurgy process, and main unit operation has: roasting, leaching, enrichment and precipitation etc.In conjunction with vanadium extraction production practice both domestic and external and research.
Sinter process is high-temperature roasting navajoite under oxidizing atmosphere, object destroys the weave construction of vanadium minerals, the lower valency vanadium in vanadium minerals is made to be oxidized to high-valence state vanadium, form the compound dissolving in acid, alkaline solution or water, therefore be an important link in the roasting process of producing at vanadium, directly have influence on the leaching yield of vanadium.Current sinter process mainly contains following several:
(1) sodium-salt calcination technique.Take NaCl as additive, at high temperature roasting, navajoite vanadium is at a middle or low price oxidized to high price soluble vanadium, then through diluted acid heap leaching and vanadium extraction, then add the direct precipitation of ammonium chloride, this is the traditional technology of vanadium extraction, by domestic and international widespread use.This method advantage is that working condition requirement is low, device simple, and cost is low, and technical process is simple, Be very effective.Shortcoming is that vanadium recovery is low, utilization of resources rate variance, and discharge macro-corrosion gas causes severe contamination to environment.
(2) calcium salt sinter process.With CaCO3, Ca (OH) 2 or CaO for additive, at high temperature mix rear roasting with navajoite, leach with diluted alkaline, leach liquor carries out ion-exchange by anionite-exchange resin, vanadium is carried out enrichment, last precipitation, domestic large quantifier elimination is made to this kind of calcium salt roasting method.This method is not only economically feasible, technically feasible, and the three wastes are easy to process, utilize, and reach free of contamination ideal effect.
(3) sinter process of composite additive, composite additive technique comprise with Na2CO3 and CaCO3 be additive, with Na2CO3 and NaCl be additive, take lime mud as additive, be additive with acid with CaO, with NaCl and MnO2 for sinter processs such as additives.
(4) take potassium permanganate as the sinter process of additive
By levigate for navajoite to 200 orders, adding bone coal amount is 10% of navajoite, mixing, and with the potassium permanganate solution group ball of 3%, roasting 8.0h, then uses the dilute sulphuric acid dump leaching of 3%, and solid-to-liquid ratio is 1:4, leaches 200h, the precipitation of chlorination money, leaching yield about 40%.This method advantage is the waste gas not producing contaminate environment in roasting process, substantially solves problem of environmental pollution, and shortcoming is that the leaching yield of vanadium is low, and the operational cycle is long.
(5) additive-free oxidizing roasting technique
By the catalyzer of the Sulphuric acid of the refinery coke of high-carbon, heavy oil ash, inefficacy, at 900 DEG C, thorough roasting makes its decarbonization, desulfuration, leaches lh at the sulphuric acid soln of 373K 2mo1/L, after solid-liquid separation, in solution, add Na2CO3, NaClO3, precipitation, the rate of recovery of vanadium reaches 83%.
Vanadium is a kind of important strategic resource, and along with the progress of science and technology, vanadium is applied to all trades and professions widely.The demand of vanadium also constantly increases in recent years, and price can be in any more especially.Therefore, from various navajoite, extract vanadium become the important developing direction of of the utilization of resources.
The vanadium resource of China is very abundant, and most of vanadium is that most low-grade navajoite is not developed fully with low-grade with other mineral paragenesis.The problems such as in silicate-type navajoite, SiO2 content is higher, when using traditional technology vanadium extraction, easily lumps when there is roasting, vanadium low conversion rate, and beneficiation enrichment is difficult, make the type ore deposit fail all the time well to develop.
The present invention is directed to silicate-type navajoite and propose a kind of process for extracting vanadium, safe production process environmental protection, the vanadium extraction rate of recovery is high.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to provide a kind of silicate-type navajoite process for extracting vanadium.Described technique have employed the Roasting And Leaching technique of one section of roasting, two sections of additive roastings, acidleach according to the feature of silicate-type navajoite, and leaching effect is good, and the leaching yield of vanadium is greater than 85%.
The present invention is by the following technical solutions:
A kind of silicate-type navajoite process for extracting vanadium, comprises baking acid immersion, ion-exchange, ammonium salt precipitation;
The Roasting And Leaching technique adopted is for being: one section of roasting, two sections of additive roastings, acidleach; One section of maturing temperature 650-750 DEG C, one section of roasting time 2.5-3.5h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 6-8%, two-stage calcination temperature 750-850 DEG C, two-stage calcination time 2.5-3.5h; 3%HCl solution leaches, extraction temperature 65-75 DEG C, extraction time 45min-75min, liquid-solid ratio 0.9-1.1:1;
The technique of employing ion-exchange is: regulate V in leach liquor 2o 5concentration is 4.5-5.5g/L, pH value is 9-11, adopts 201 × 7 exchange resins to carry out extraction to the vanadium in leach liquor and reclaims; Employing NaCl content 9-11%, pH value are that the elutriant of 9-11 carries out desorb.
Preferably, the Roasting And Leaching technique of employing is for being: one section of roasting, two sections of additive roastings, acidleach; One section of maturing temperature 700 DEG C, one section of roasting time 3h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 7%, two-stage calcination temperature 800 DEG C, two-stage calcination time 3h; 3%HCl solution leaches, extraction temperature 70 DEG C, extraction time lh, liquid-solid ratio 1:1, and the leaching yield that can obtain vanadium is greater than 85%;
Preferably, the technique of employing ion-exchange is: regulate V in leach liquor 2o 5concentration is 5.02g/L, pH value is 10.0, adopts 201 × 7 exchange resins to carry out extraction to the vanadium in leach liquor and reclaims; Adopt NaCl content 10%, pH value be 10.0 elutriant carry out desorb.
Preferably, in order to reach desirable ion-exchange effect, need pre-treatment be carried out to resin and carry out purifying treatment to containing vanadium solution:
(1) pre-treatment of resin: because synthetic resins situation more complicated, often with side reaction, make containing part oils or organism in rosin products, a little iron contamination, can affect the effect of ion-exchange, must carry out suitable purifying treatment to resin in addition.Resin is placed in exchange column, first rinse by 3-5% hydrochloric acid acid solution, again with clear water by resin drip washing to neutral, then clean with the sodium hydroxide buck of 5-10%, use clear water drip washing to neutral afterwards again, continuous agitating resin in process, after placing 1-2h, repeat this process more once, after handling well, resin being placed on temperature is dry in 40-60 DEG C of baking oven.
(2) purifying treatment of leach liquor: under different acidity, there is different states in vanadium, therefore, the method that must neutralize according to the kind employing of resin used or dilute regulates the pH value containing vanadium solution in the solution.If there is potassium permanganate to exist in vanadium solution, it can destroy resin property, in order to eliminate its impact on resin, potassium permanganate need be changed into Manganse Dioxide.Consider exchange capacity and the exchange selectivity of resin, carry out resins exchange with rare vanadium solution better.Heat in process, avoid producing colloid or precipitation.If produce colloid or precipitation in solution, then can covering resin surface, can block resin layer, make flow velocity slack-off, serious words even can not exchange.
The present invention is described in detail below:
Silicate-type navajoite is based on silicate, and in silicate, vanadium is with V 3+isomorph form replaces the A1 of 6 coordinations 3+and be present in mica lattice, must break ring micaceous structure, making it oxidation just can stripping.Carbon containing in this ore, causes calcination atmosphere and is in reductibility, is unfavorable for that lower valency vanadium is oxidized.Directly or add additive and be mixed in high-temperature roasting under oxidizing atmosphere, all there is lower valency vanadium and be difficult to be oxidized or to be converted into the problems such as the Vanadium Pentoxide in FLAKES that is beneficial to leaching or vanadate in navajoite.
When maturing temperature is lower, mineral structure fails to destroy completely, and the oxidation of Low Valent Vanadium is incomplete, causes leaching yield low; Maturing temperature is too high, likely reaches the fusing point of low melting point ore, causes mineral surface clinkering, hinders the diffusion of oxygen, causes transformation efficiency to decline equally.Roasting time or baking inphases can be extended, strengthen gas velocity, be conducive to improving transformation efficiency.Improve the leaching yield of vanadium, suitable roasting scheme, maturing temperature and roasting time be selected.
Therefore the present invention is through a large amount of Roasting And Leaching technique determining use one section of roasting, two sections of additive roastings, acidleach, under the condition of optimum: one section of maturing temperature 700 DEG C, one section of roasting time 3h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 7%, two-stage calcination temperature 800 DEG C, two-stage calcination time 3h; 3%HCl solution leaches, and extraction temperature 70 DEG C, extraction time lh, liquid-solid ratio 1:1, the leaching yield of vanadium is greater than 85%.
The present invention has the following advantages: the present invention have employed the Roasting And Leaching technique of one section of roasting, two sections of additive roastings, acidleach according to the feature of silicate-type navajoite, and leaching effect is good, and the leaching yield of vanadium is greater than 85%.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment one
A kind of silicate-type navajoite process for extracting vanadium, comprises baking acid immersion, ion-exchange, ammonium salt precipitation;
The Roasting And Leaching technique adopted is for being: one section of roasting, two sections of additive roastings, acidleach; One section of maturing temperature 700 DEG C, one section of roasting time 3h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 7%, two-stage calcination temperature 800 DEG C, two-stage calcination time 3h; 3%HCl solution leaches, extraction temperature 70 DEG C, and extraction time lh, liquid-solid ratio 1:1, can obtain the leaching yield complete 85% of vanadium;
The technique of employing ion-exchange is: regulate V in leach liquor 2o 5concentration is 5.02g/L, pH value is 10.0, adopts 201 × 7 exchange resins to carry out extraction to the vanadium in leach liquor and reclaims; Adopt NaCl content 10%, pH value be 10.0 elutriant carry out desorb.Resin carries out pre-treatment: be placed on by resin in exchange column, first rinse by 3-5% hydrochloric acid acid solution, again with clear water by resin drip washing to neutral, then clean with the sodium hydroxide buck of 5-10%, use clear water drip washing to neutral afterwards again, continuous agitating resin in process, after placing 1-2h, repeat this process more once, after handling well, resin being placed on temperature is dry in 40-60 DEG C of baking oven.
Embodiment two
A kind of silicate-type navajoite process for extracting vanadium, comprises baking acid immersion, ion-exchange, ammonium salt precipitation;
The Roasting And Leaching technique adopted is for being: one section of roasting, two sections of additive roastings, acidleach; One section of maturing temperature 650 DEG C, one section of roasting time 2.5h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 6%, two-stage calcination temperature 750 DEG C, two-stage calcination time 2.5h; 3%HCl solution leaches, extraction temperature 65 DEG C, extraction time 45min, liquid-solid ratio 0.9:1;
The technique of employing ion-exchange is: regulate V in leach liquor 2o 5concentration is 4.5g/L, pH value is 9, adopts 201 × 7 exchange resins to carry out extraction to the vanadium in leach liquor and reclaims; Adopt NaCl content 9%, pH value be 9 elutriant carry out desorb.Resin carries out pre-treatment: be placed on by resin in exchange column, first rinse by 3-5% hydrochloric acid acid solution, again with clear water by resin drip washing to neutral, then clean with the sodium hydroxide buck of 5-10%, use clear water drip washing to neutral afterwards again, continuous agitating resin in process, after placing 1-2h, repeat this process more once, after handling well, resin being placed on temperature is dry in 40-60 DEG C of baking oven.
Embodiment three
A kind of silicate-type navajoite process for extracting vanadium, comprises baking acid immersion, ion-exchange, ammonium salt precipitation;
The Roasting And Leaching technique adopted is for being: one section of roasting, two sections of additive roastings, acidleach; One section of maturing temperature 750 DEG C, one section of roasting time 3.5h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 8%, two-stage calcination temperature 850 DEG C, two-stage calcination time 3.5h; 3%HCl solution leaches, extraction temperature 75 DEG C, extraction time 75min, liquid-solid ratio 1.1:1;
The technique of employing ion-exchange is: regulate V in leach liquor 2o 5concentration is 5.5g/L, pH value is 11, adopts 201 × 7 exchange resins to carry out extraction to the vanadium in leach liquor and reclaims; Adopt NaCl content 11%, pH value be 11 elutriant carry out desorb.Resin carries out pre-treatment: be placed on by resin in exchange column, first rinse by 3-5% hydrochloric acid acid solution, again with clear water by resin drip washing to neutral, then clean with the sodium hydroxide buck of 5-10%, use clear water drip washing to neutral afterwards again, continuous agitating resin in process, after placing 1-2h, repeat this process more once, after handling well, resin being placed on temperature is dry in 40-60 DEG C of baking oven.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.

Claims (5)

1. a silicate-type navajoite process for extracting vanadium, comprises baking acid immersion, ion-exchange, ammonium salt precipitation;
The Roasting And Leaching technique adopted is for being: one section of roasting, two sections of additive roastings, acidleach; One section of maturing temperature 650-750 DEG C, one section of roasting time 2.5-3.5h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 6-8%, two-stage calcination temperature 750-850 DEG C, two-stage calcination time 2.5-3.5h; 3%HCl solution leaches, extraction temperature 65-75 DEG C, extraction time 45min-75min, liquid-solid ratio 0.9-1.1:1;
The technique of employing ion-exchange is: regulate V in leach liquor 2o 5concentration is 4.5-5.5g/L, pH value is 9-11, adopts 201 × 7 exchange resins to carry out extraction to the vanadium in leach liquor and reclaims; Employing NaCl content 9-11%, pH value are that the elutriant of 9-11 carries out desorb.
2. technique according to claim 1, preferably, the Roasting And Leaching technique of employing is for being: one section of roasting, two sections of additive roastings, acidleach; One section of maturing temperature 700 DEG C, one section of roasting time 3h, navajoite grinding particle size-200 order 80%; Two-stage calcination sodium carbonate 7%, two-stage calcination temperature 800 DEG C, two-stage calcination time 3h; 3%HCl solution leaches, and extraction temperature 70 DEG C, extraction time lh, liquid-solid ratio 1:1, the leaching yield that can obtain vanadium is greater than 85%.
3. technique according to claim 1, preferably, the technique of employing ion-exchange is: regulate V in leach liquor 2o 5concentration is 5.02g/L, pH value is 10.0, adopts 201 × 7 exchange resins to carry out extraction to the vanadium in leach liquor and reclaims; Adopt NaCl content 10%, pH value be 10.0 elutriant carry out desorb.
4. technique according to claim 1, preferably, in order to reach desirable ion-exchange effect, need carry out pre-treatment to resin and carry out purifying treatment to containing vanadium solution.
5. technique according to claim 4, the pre-treatment of resin is: first rinse by 3-5% hydrochloric acid acid solution, again with clear water by resin drip washing to neutral, then clean with the sodium hydroxide buck of 5-10%, use clear water drip washing to neutral afterwards again, continuous agitating resin in process, after placing 1-2h, repeat this process more once, after handling well, resin being placed on temperature is dry in 40-60 DEG C of baking oven.
CN201310299567.9A 2013-07-16 2013-07-16 Vanadium extracting process for silicate type vanadium ore Pending CN104294033A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106011456A (en) * 2016-08-02 2016-10-12 北京科技大学 Method for enrichment of vanadium in vanadium-containing stone coal and V-concentrating phase regulation
CN107805710A (en) * 2017-10-23 2018-03-16 中国科学院过程工程研究所 A kind of method of the silicate mineral synthetical recovery silicon of vanadium containing multivalent state and vanadium
CN108034807A (en) * 2017-12-08 2018-05-15 湖南三丰钒业有限公司 A kind of transforming agent and its application method for being used for the vanadium extraction from vanadium raw ore
CN108251661A (en) * 2018-01-30 2018-07-06 长春师范大学 A kind of bone coal navajoite process for extracting vanadium

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106011456A (en) * 2016-08-02 2016-10-12 北京科技大学 Method for enrichment of vanadium in vanadium-containing stone coal and V-concentrating phase regulation
CN107805710A (en) * 2017-10-23 2018-03-16 中国科学院过程工程研究所 A kind of method of the silicate mineral synthetical recovery silicon of vanadium containing multivalent state and vanadium
CN107805710B (en) * 2017-10-23 2019-03-12 中国科学院过程工程研究所 A method of the silicate mineral synthetical recovery silicon of vanadium containing multivalent state and vanadium
CN108034807A (en) * 2017-12-08 2018-05-15 湖南三丰钒业有限公司 A kind of transforming agent and its application method for being used for the vanadium extraction from vanadium raw ore
CN108251661A (en) * 2018-01-30 2018-07-06 长春师范大学 A kind of bone coal navajoite process for extracting vanadium

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Application publication date: 20150121