CN108754125B - Clean process for extracting vanadium from vanadium-containing material through sodium salt roasting - Google Patents
Clean process for extracting vanadium from vanadium-containing material through sodium salt roasting Download PDFInfo
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Abstract
The invention relates to a sodium salt roasting vanadium extraction cleaning process of vanadium-containing materials, which comprises the steps of adding sodium chloride into vanadium-containing material ores, uniformly mixing and grinding, roasting ores, removing harmful gases in roasted flue gas by using an adsorbent, discharging the roasted flue gas after reaching the standard, leaching the obtained roasted sand by water and then alkaline leaching, leaching the roasted sand by adding water, filtering to obtain a water leaching solution and water leaching slag, leaching the water leaching slag by adding a sodium carbonate solution, filtering to obtain an alkaline leaching solution and leaching slag, adding calcium chloride into the water leaching solution to precipitate and enrich vanadium, filtering to obtain a calcium vanadate filter cake and a vanadium precipitation solution, returning the vanadium precipitation solution to a roasted sand water leaching process or a vanadium-containing material ore mixing or ore agglomeration process for recycling, decomposing the obtained calcium vanadate filter cake by using an alkaline leaching solution, filtering to obtain calcium carbonate and vanadium enrichment solution, calcining the calcium carbonate to convert into calcium oxide, returning to a high-temperature flue gas purification process, crystallizing the vanadium from the vanadium enrichment solution by adding ammonium salt to precipitate, filtering to obtain ammonium, the crystallization mother liquor is directly returned to the alkaline leaching process, or returned to the alkaline leaching process for recycling after calcium is added to precipitate vanadium. The sodium chloride, the lime, the sodium carbonate salt and the water are recycled in the process, and the method has the advantages of simple process, high vanadium recovery rate, low production cost, cleanness, environmental protection and the like.
Description
Technical Field
The invention relates to a clean process for extracting vanadium by sodium salt roasting of a vanadium-containing material.
Background
The vanadium slag and the stone coal are vanadium-containing materials which are main raw materials for producing vanadium pentoxide.
Vanadium in the vanadium slag mainly exists in a spinel form, and the main production process for extracting vanadium from the vanadium slag at present comprises the steps of sodium roasting of the vanadium slag, water leaching, purification, precipitation of vanadium from weak acid ammonium salt and thermal decomposition of ammonium polyvanadate to obtain a vanadium pentoxide product. And (3) reducing the solution after vanadium precipitation, neutralizing and precipitating vanadium and chromium, and evaporating and concentrating the solution after precipitation to obtain a mixture of ammonium sulfate/sodium chloride. The treatment process of the vanadium precipitation post-liquid generated by the vanadium slag sodium salt roasting vanadium extraction process is complex and high in production cost, and the generated vanadium-chromium reduction slag and the mixture of ammonium sulfate/sodium chloride containing vanadium and chromium are dangerous solid wastes.
The vanadium in the stone coal is mainly low-valence vanadium which exists in the mica in the same-phase-like form, and the vanadium must be dissociated from the mica crystal phase for extracting the vanadium from the stone coal.
The vanadium extraction process from stone coal can be roughly divided into acid leaching process, alkaline leaching process and sodium roasting-water leaching process, and the processes have advantages and disadvantages respectively. The leaching rate of vanadium in the stone coal acid leaching vanadium extraction process is high and can reach 80-90%, but the acid utilization rate in the leaching process is low, a large amount of impurities enter a solution, the leaching residue has poor liquid-solid separation performance, and the treatment difficulty of waste water and waste residue generated in the stone coal vanadium extraction is high. The process for extracting vanadium from stone coal by alkaline leaching is only suitable for extracting vanadium from stone coal with more alkaline gangue, vanadium in the stone coal must be oxidized into pentavalent vanadium before alkaline leaching, the requirements of stone coal oxidizing roasting on roasting temperature and atmosphere are strict, and the industrial production cannot meet the process requirements easily. The sodium roasting-water leaching vanadium process is a traditional process for extracting vanadium from stone coal, and comprises the following process steps: the method comprises the steps of stone coal sodium roasting, water leaching, ion exchange, weak base ammonium salt vanadium precipitation and ammonium metavanadate thermal decomposition of vanadium pentoxide products. The vanadium-containing material is subjected to a sodium roasting-water leaching vanadium process, and the leaching rate of vanadium is low and is only 50-60% generally. Flue gas generated by sodium roasting of vanadium-containing materials is sprayed and absorbed by alkali liquor to reach the standard and discharged, but the cost is higher, a large amount of salt-containing waste water and waste residue are generated, vanadium in the leaching solution is enriched by ion exchange, and Cl is used-Competition of ions, Cl in the feed liquid-The higher the ion, the smaller the exchange capacity of the resin to V, so the feed liquid must be diluted before exchange, and the post-exchange liquid can not be returned for continuous use and can only be discharged outside, thereby generating a large amount of salt-containing wastewater, which not only causes the giving expense of sodium chloride resources, but also causes environmental pollution.
Disclosure of Invention
The invention aims to reduce the production cost of vanadium extraction from vanadium-containing materials and protect the environment, and provides a clean process for extracting vanadium from vanadium-containing materials by sodium roasting.
The invention relates to a clean process for extracting vanadium by sodium salt roasting of vanadium-containing materials, which comprises the following steps:
the first step is as follows: after the calcine obtained by sodium salt roasting of the vanadium-containing material is soaked in water, calcium is added into the water leaching solution to precipitate and enrich vanadium, and calcium vanadate filter cake and vanadium-precipitated solution are obtained after filtration; carrying out alkaline leaching on the water leaching residue by using sodium carbonate solution, and filtering to obtain vanadium-containing alkaline leaching solution and alkaline leaching residue; the second step is that: decomposing the obtained calcium vanadate filter cake by using vanadium-containing alkali immersion liquid, filtering to obtain a calcium vanadate filter cake and a vanadium enrichment liquid, concentrating all vanadium in the calcine water immersion liquid and the alkali immersion liquid into the vanadium enrichment liquid, and adding ammonium salt into the obtained vanadium enrichment liquid to precipitate vanadium.
The invention relates to a clean process for sodium salt roasting vanadium extraction of a vanadium-containing material, which comprises the steps of adding calcium precipitation to enrich vanadium in the first step, wherein the calcium precipitation is that a calcium-containing compound is added according to 0.8-1.2 times of the stoichiometric number of the vanadium in a water leaching solution converted into calcium vanadate, the calcium-containing compound is selected from calcium chloride or/and calcium oxide or/and calcium hydroxide, the reaction is carried out for 0.5-2.5 h at the temperature of 0-100 ℃, preferably for 1-1.5 h at the temperature of 40-60 ℃, filtering is carried out to obtain a calcium vanadate filter cake and a vanadium precipitation liquid, the vanadium precipitation liquid returns to a calcine water leaching process or a vanadium-containing material agglomeration process as a raw material for recycling, and the added calcium chloride is preferably calcium chloride obtained by high.
The invention relates to a clean process for extracting vanadium from vanadium-containing materials by sodium salt roasting, wherein the vanadium precipitation of ammonium salt refers to that ammonium carbonate or ammonium bicarbonate or ammonium chloride is added according to the proportion of 0.7-1.3 times of the stoichiometric number of the vanadium in a vanadium enrichment solution to the ammonium metavanadate, so that vanadium in the vanadium enrichment solution is crystallized and separated out, the ammonium metavanadate and a crystallization mother solution thereof are obtained by filtering, and the crystallization mother solution is directly returned to an alkaline leaching process for recycling, or calcium oxide or calcium hydroxide is added firstly to precipitate vanadium and then returned to the alkaline leaching process for recycling.
The invention relates to a clean process for extracting vanadium by sodium salt roasting of a vanadium-containing material.
In the first step, alkaline leaching refers to adding water leaching residues into 0.5-2.5 mol/L of sodium carbonate solution according to a solid-to-liquid ratio of 1: 1-4 g/m L, leaching for 1-5 hours at 0-100 ℃, preferably leaching for 2-3 hours at 25-65 ℃, and filtering to obtain alkaline leaching solution and alkaline leaching residues.
The invention relates to a clean process for extracting vanadium by sodium salt roasting of a vanadium-containing material, which comprises the first step of leaching vanadium from water leaching slag in an alkaline leaching way to ensure that the total leaching rate of vanadium in calcine reaches 80-95%.
In the second step, the alkaline leaching solution decomposition refers to mixing a calcium vanadate filter cake and the vanadium-containing alkaline leaching solution, stirring or ball milling for 0.5-5 h at 0-100 ℃, preferably stirring and ball milling for 1-2 h at room temperature, allowing vanadium in the calcium vanadate filter cake to enter a solution, and filtering to obtain a calcium carbonate and vanadium enrichment solution.
The invention relates to a clean process for extracting vanadium by sodium salt roasting of a vanadium-containing material, wherein a vanadium-precipitated liquid obtained in the first step is returned to an ore agglomeration procedure or a calcine water leaching procedure of the process for extracting vanadium by sodium salt roasting of the vanadium-containing material for recycling;
the calcium carbonate obtained in the second step is directly returned to be used as a raw material for purifying the vanadium-containing material sodium salt roasting flue gas or returned to be used as a raw material for purifying the flue gas for recycling after being calcined and converted into calcium oxide;
the ammonium salt vanadium precipitation is to add ammonium salt into the vanadium enrichment solution to crystallize and separate out vanadium, filter to obtain ammonium metavanadate and crystallization mother liquor thereof, and thermally decompose the ammonium metavanadate to obtain a vanadium pentoxide product; the crystallization mother liquor is directly returned to the water leaching residue alkaline leaching process for recycling, or is returned to the water leaching residue alkaline leaching process for recycling after calcium is added to precipitate vanadium.
The invention relates to a clean process for extracting vanadium by sodium salt roasting of a vanadium-containing material, wherein the vanadium-containing material comprises vanadium slag and stone coal;
the sodium salt roasting of the vanadium-containing material is to add sodium chloride or/and sodium carbonate into the vanadium-containing material or the pre-decarbonization vanadium-containing material, finely grind, mix and roast, or finely grind, mix, agglomerate and roast; the amount of sodium chloride and sodium carbonate is 5-25% of the mass of the vanadium-containing material ore, wherein the mass ratio of sodium chloride to sodium carbonate is 1-100.
The invention relates to a vanadium-containing material sodium salt roasting vanadium extraction cleaning process, wherein flue gas generated by the vanadium-containing material sodium salt roasting is directly absorbed and removed with an adsorbent in a dry method, or the adsorbent and a water mixture are sprayed and absorbed to remove the harmful gas, so that the purified flue gas reaches the standard and is discharged; the adsorbent is at least one selected from calcium oxide, calcium hydroxide and calcium carbonate; chlorine-containing gas in the flue gas in the purification process reacts with the adsorbent and then is converted into calcium chloride.
The invention relates to a clean process for extracting vanadium by sodium salt roasting of a vanadium-containing material, which comprises the steps of adding water into roasted sand according to a solid-to-liquid ratio of 1: 1-5 g/m L, leaching for 1-10 h at 0-100 ℃, preferably leaching for 2-3 h at room temperature, and filtering to obtain a water leaching solution and water leaching slag.
The specific technological process implemented by the invention is as follows:
the process flow is as shown in figure 1, and mainly comprises the following steps of carrying out sodium salt roasting on a vanadium-containing material, purifying flue gas, carrying out water leaching on roasted sand and then carrying out alkali leaching, adding calcium to enrich vanadium into a water leaching solution, decomposing a calcium vanadate alkali leaching solution, precipitating vanadium from an ammonium salt of the vanadium-enriched solution, carrying out thermal hydrolysis on ammonium metavanadate to obtain a vanadium pentoxide product, adding 5-20% of sodium chloride into the vanadium-containing material mineral powder, uniformly mixing and grinding the mixture to-100 meshes, roasting the mixture at 700-850 ℃ for 1-4 hours, adding water into the roasted sand according to a solid-to-liquid ratio of 1: 1-5 g/m L, leaching the roasted sand at 0-100 ℃ for 1-10 hours, filtering to obtain a water leaching solution and water leaching residue, adding the water leaching residue into a sodium carbonate solution at a solid-to-liquid ratio of 1: 1-4 g/m L, leaching for 1-2.5 mol/m of L, leaching the solution at 0-100 ℃ for 1-5 hours, filtering to obtain a vanadium-containing alkali leaching solution and a vanadium-leaching solution and a filtering to obtain a vanadium-containing calcium carbonate leaching solution, carrying out a calcium hydroxide leaching solution, carrying out a circular ball-leaching process, and a calcium carbonate leaching process, filtering the calcium carbonate leaching solution, and a calcium hydroxide leaching process of the calcium carbonate leaching solution, wherein the calcium carbonate leaching solution is used for converting the calcium carbonate leaching solution into a calcium carbonate leaching solution, and a calcium carbonate leaching process of calcium hydroxide, and a calcium carbonate leaching process of calcium metavanadate, and a calcium hydroxide, and a calcium carbonate leaching process of calcium hydroxide, wherein the calcium carbonate, and a filter cake, and a calcium carbonate leaching process is carried out circular leaching process of calcium hydroxide, and a filter cake, and a circular leaching process of calcium carbonate, wherein the calcium carbonate, the.
The process provided by the invention can effectively extract vanadium in vanadium-containing materials to prepare V with the metallurgical grade of more than 982O5The product can realize sodium chloride, calcium chloride, sodium carbonate, lime and waterThe method has the advantages of simple process, high vanadium recovery rate, low production cost, cleanness, environmental protection and the like.
Compared with the prior art, the invention has the following advantages and effects:
1. calcium chloride is added into the water leaching solution to precipitate and enrich vanadium, so that Cl in the leaching solution is ingeniously broken-The difficult problem that ion accumulation interferes with vanadium separation and enrichment can be solved, chemical raw materials such as sodium chloride and the like can be recycled in the process without evaporation and concentration, and the process is simple and environment-friendly.
2. The calcine is subjected to water leaching and then alkali leaching, so that the leaching rate of vanadium in low-grade vanadium-containing materials such as stone coal is improved to 80-95% from 60-70%, the obtained vanadium-containing alkali leaching solution is mixed with a calcium vanadate filter cake, the separation of vanadium and calcium is realized, the vanadium is further purified and enriched, and the improvement of the yield of the vanadium and the product quality are facilitated.
3. By means of the cyclic conversion of calcium oxide → calcium chloride → calcium vanadate → calcium carbonate → calcium oxide, a cyclic metallurgy process flow for extracting vanadium by sodium salt roasting of the vanadium-containing material is formed, the cyclic utilization of sodium chloride, lime, sodium carbonate salt and water in the process flow is realized, and the process flow for extracting vanadium from the vanadium-containing material is clean and environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention will now be further described with reference to the following examples, which are intended to illustrate the invention but not to limit it further.
Example 1
Adding 600g of sodium chloride into 10kg of a pre-decarbonized stone coal mine containing 0.95% of vanadium (V), uniformly mixing and grinding the pre-decarbonized stone coal mine into-120-mesh agglomerates, roasting the pre-decarbonized stone coal mine for 2.5h at 750 ℃, absorbing harmful gas in roasting smoke gas by using a phi 10-15 lime ball filtering layer, adding water into calcine according to a solid-liquid ratio of 1:2g/m L to leach for 3h at room temperature, filtering the calcine to obtain a water leaching solution and water leaching slag, adding a sodium carbonate solution of 1 mol/L into the water leaching slag according to a solid-liquid ratio of 1:2.5g/m L, stirring and leaching the water leaching slag for 3h at 25 ℃, filtering to obtain an alkali leaching solution and leaching slag, wherein the leaching slag contains 0.15% of vanadium (V) and the total leaching rate of vanadium is 84.5%, converting the water leaching solution into 1 time of chemical metering amount of calcium vanadate, adding calcium chloride, stirring the calcium chloride at room temperature for 0.5h, filtering to obtain a calcium vanadate filter cake and a post-precipitation solution, stirring and adding a calcium vanadate filter cake into a vanadium carbonate enrichment solution according to obtain a vanadium carbonate and a vanadium carbonate crystallization concentrate, pyrolyzing a ammonium metavanadate crystal at room temperature to obtain a vanadium metavanadate crystal, adding a crystal, and adding a crystal concentrate, and adding a crystal seed crystal with.
Example 2
Adding 150g of sodium chloride into 5kg of stone coal mineral powder (minus 150 meshes) containing 1.13% of vanadium (V), roasting the vanadium-precipitated agglomerated ore obtained in the embodiment 1 at 790 ℃ for 2h, absorbing harmful gas in the roasted flue gas by a phi 10-15 lime ball filter layer, adding the roasted sand into the vanadium-precipitated liquid chamber obtained in the embodiment 1 according to the solid-to-liquid ratio of 1:2g/m L, carrying out warm leaching for 2.5h, filtering to obtain a water leaching solution and water leaching slag, adding the water leaching slag into the crystallization mother liquor obtained in the embodiment 1 according to the solid-to-liquid ratio of 1:3g/m L, carrying out stirring leaching at 80 ℃ for 1.5h, filtering to obtain an alkali leaching solution and leaching slag, wherein the leaching slag (V) is 0.093%, the total leaching rate of vanadium is 91.8%, converting the vanadium contained in the water leaching solution into 1 time of the stoichiometric number of calcium vanadate, adding the calcium chloride containing a small amount of calcium oxide obtained in the embodiment 1 by high-temperature purification of the vanadium-containing vanadium, stirring for 1.5h, filtering to obtain calcium vanadate, adding the calcium vanadate and vanadium-precipitated liquid into the calcium chloride-precipitated calcium-vanadium-precipitated liquid, carrying out thermal decomposition, adding the calcium-vanadium-enriched calcium chloride-enriched calcium chloride-enriched calcium-.
Example 3
Adding 60g of sodium carbonate and 40g of sodium chloride into 500g of vanadium slag containing 13.5% of vanadium (V), grinding, uniformly mixing, roasting at 800 ℃ for 3h, adding water into the roasted product according to a solid-to-liquid ratio of 1:3g/m L for 2.5h, filtering to obtain a water leaching solution and water leaching slag, adding 1.5 mol/L of sodium carbonate solution into the water leaching slag according to a solid-to-liquid ratio of 1:2.5g/m L, stirring and leaching at 65 ℃ for 2h, filtering to obtain an alkali leaching solution and leaching slag, wherein the vanadium-containing slag contains 0.57% of vanadium (V) and the total leaching rate of vanadium is 95.9%, converting the vanadium in the water leaching solution into a mixture of calcium vanadate and calcium chloride with a stoichiometric number of 1.2 times that of the mixture, stirring and ball-milling at room temperature for 1.5h, filtering to obtain a calcium vanadate and vanadium-precipitated solution, stirring and adding a calcium vanadate filter cake into the alkali leaching solution, stirring and filtering to obtain a vanadium metavanadate crystal cake, wherein the ammonium metavanadate crystal is obtained by adding ammonium metavanadate crystal seed crystals with a purity of 550 ℃ and ammonium metavanadate crystals with a purity of 3 h.
Claims (10)
1. A clean process for extracting vanadium by sodium salt roasting of stone coal comprises the following steps:
the first step is as follows: after the calcine obtained by the sodium roasting of the stone coal is soaked in water, calcium chloride is added into the water leaching solution to precipitate and enrich vanadium, and a calcium vanadate filter cake and a solution after vanadium precipitation are obtained by filtering; carrying out alkaline leaching on the water leaching residue by using sodium carbonate solution, and filtering to obtain vanadium-containing alkaline leaching solution and alkaline leaching residue; the sodium salt roasting of the stone coal is to add sodium chloride into the stone coal or the pre-decarbonized stone coal to be levigated, uniformly mixed and roasted, or levigated, uniformly mixed, agglomerated and roasted; the solution after vanadium precipitation is returned to the agglomeration procedure or calcine water leaching procedure of the stone coal sodium salt roasting vanadium extraction process for recycling; flue gas generated by sodium roasting of the stone coal is directly absorbed and removed with an adsorbent in a dry method, or the adsorbent and water mixture is sprayed to absorb and remove the harmful gas, so that the flue gas is purified and then discharged after reaching the standard; the adsorbent is at least one selected from calcium oxide, calcium hydroxide and calcium carbonate;
the second step is that: decomposing the obtained calcium vanadate filter cake by using vanadium-containing alkali immersion liquid, filtering to obtain a calcium vanadate filter cake and a vanadium enrichment solution, adding ammonium salt into the obtained vanadium enrichment solution to precipitate vanadium, and filtering to obtain ammonium metavanadate and a crystallization mother solution thereof; the crystallization mother liquor is directly returned to the water leaching residue alkaline leaching process for recycling, or returned to the water leaching residue alkaline leaching process for recycling after calcium is added for vanadium precipitation; the obtained calcium carbonate is directly returned to be used as a raw material for purifying the stone coal sodium salt roasting smoke or returned to be used as a raw material for purifying the smoke after being calcined and converted into calcium oxide for recycling.
2. The stone coal sodium salt roasting vanadium extraction cleaning process according to claim 1, characterized in that: in the first step, calcium chloride is added to precipitate and enrich vanadium, namely, calcium chloride is added according to the stoichiometric number of 0.8-1.2 times of that of vanadium in the water extract converted into calcium vanadate, the calcium chloride reacts for 0.5-2.5 hours at the temperature of 0-100 ℃, and calcium vanadate filter cakes and a vanadium precipitation solution are obtained through filtration.
3. The stone coal sodium salt roasting vanadium extraction cleaning process according to claim 1, characterized in that: in the first step, the sodium carbonate solution added to the water-immersed residue is at least one of a sodium carbonate solution and a sodium bicarbonate solution.
4. The clean process for extracting vanadium by sodium salt roasting of stone coal as claimed in claim 3, wherein in the first step, the alkaline leaching is to add water leaching residue into 0.5-2.5 mol/L of sodium carbonate solution according to a solid-to-liquid ratio of 1: 1-4 g/m L, leach for 1-5 h at 0-100 ℃, and filter to obtain vanadium-containing alkaline leaching solution and alkaline leaching residue.
5. The stone coal sodium salt roasting vanadium extraction cleaning process according to claim 4, characterized in that: after alkaline leaching of the water leaching residue, the total leaching rate of vanadium in the calcine reaches 80-95%.
6. The process for extracting vanadium from stone coal by sodium salt roasting according to any one of claims 1 to 4, wherein: in the second step, the alkaline leaching solution decomposition means that a calcium vanadate filter cake is mixed with the vanadium-containing alkaline leaching solution, and the mixture is stirred or ball-milled for 0.5 to 5 hours at the temperature of 0 to 100 ℃ so that vanadium in the mixture enters the solution, and the calcium carbonate and vanadium enrichment solution is obtained by filtering.
7. The stone coal sodium salt roasting vanadium extraction cleaning process as claimed in claim 6, characterized in that:
the ammonium salt vanadium precipitation is to add ammonium salt into the vanadium enrichment solution to crystallize and separate out vanadium, filter to obtain ammonium metavanadate and crystallization mother liquor thereof, and thermally decompose the ammonium metavanadate to obtain a vanadium pentoxide product; the crystallization mother liquor is directly returned to the water leaching residue alkaline leaching process for recycling, or is returned to the water leaching residue alkaline leaching process for recycling after calcium is added to precipitate vanadium.
8. The stone coal sodium salt roasting vanadium extraction cleaning process according to claim 7, characterized in that: the ammonium salt vanadium precipitation means that ammonium carbonate, ammonium bicarbonate or ammonium chloride is added according to the stoichiometric number of 0.7-1.3 times of the amount of the vanadium in the vanadium enrichment solution converted into ammonium metavanadate.
9. The stone coal sodium salt roasting vanadium extraction cleaning process according to claim 8, characterized in that:
and (3) carrying out sodium modification roasting on the stone coal, wherein the amount of sodium chloride is 5-20% of the mass of the stone coal mine.
10. The clean process for extracting vanadium by sodium salt roasting of stone coal as claimed in claim 9, wherein in the sodium salt roasting process of stone coal, water leaching is carried out by adding water into roasted sand according to a solid-to-liquid ratio of 1: 1-5 g/m L, leaching for 1-10 h at 0-100 ℃, and filtering to obtain water leaching solution and water leaching slag.
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