CN110358909B - Method for green and efficient utilization of carbon in high-carbon vanadium-containing stone coal and pre-enrichment of vanadium - Google Patents

Method for green and efficient utilization of carbon in high-carbon vanadium-containing stone coal and pre-enrichment of vanadium Download PDF

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CN110358909B
CN110358909B CN201910648178.XA CN201910648178A CN110358909B CN 110358909 B CN110358909 B CN 110358909B CN 201910648178 A CN201910648178 A CN 201910648178A CN 110358909 B CN110358909 B CN 110358909B
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闫柏军
刘坤鹏
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University of Science and Technology Beijing USTB
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Abstract

A method for green and efficient utilization of carbon and pre-enrichment of vanadium in high-carbon vanadium-containing stone coal belongs to the field of comprehensive utilization of resources. The method comprises the following steps: using high-carbon vanadium-containing coal mine as raw material, Fe2O3As an additive, MgO or Al2O3As modifier, the raw materials are crushed and fully mixed with additive and modifier to prepare pellets. After drying, the carbon in the high-carbon stone coal is gasified by adopting water vapor and then roasted, and vanadium-containing enriched phase-vanadium iron spinel can be generated in the product. And crushing, grinding and magnetically separating to obtain vanadium-containing concentrate with low impurity content and high vanadium grade. The method has the advantages of high resource utilization rate, energy conservation, environmental protection, high carbon gasification and vanadium enrichment efficiency and the like. The method can convert carbon resources in the high-carbon stone coal into clean energy in an environment-friendly and efficient manner, can obtain a vanadium-rich phase with high vanadium content and is convenient to separate, can treat the high-carbon vanadium-containing stone coal resources in an environment-friendly and efficient manner, and has important significance for comprehensive utilization of the stone coal resources.

Description

Method for green and efficient utilization of carbon in high-carbon vanadium-containing stone coal and pre-enrichment of vanadium
Technical Field
The invention belongs to the technical field of utilization of high-carbon vanadium-containing stone coal carbon resources and vanadium pre-enrichment, and particularly relates to a method for pre-enriching vanadium resources in high-carbon stone coal to obtain vanadium-rich concentrate with high vanadium grade, and converting the carbon resources in the vanadium-rich concentrate into clean energy. The method can be used for green and high-efficiency treatment of high-carbon vanadium-containing stone coal resources, and has important significance for comprehensive utilization of the stone coal resources.
Background
Vanadium is a transition metal, and metal vanadium, vanadium compounds and vanadium alloys are widely used in various fields of society due to its excellent physicochemical properties. The vanadium-containing minerals in China are more, and the distribution is wider, and the reserves are huge. However, there are two main types of vanadium ore with high industrial utilization value, namely, stone coal and vanadium titano-magnetite. The vanadium-containing stone coal mine is widely distributed in southern provinces of China, and V stored in stone coal2O5Occupies V in vanadium ore of China2O587% of the total reserves, and therefore of great significance for their utilization. The high-carbon vanadium-containing stone coal mainly contains SiO2、C、Al2O3And a small amount of K2O, MgO and V2O3. The carbon content of the vanadium-containing stone coal mineral in China is generally 10-15%, the vanadium content is low, and V is2O5Grade (L) of a materialMostly 0.3-1%, mainly existing in the vanadium mica ore and comparatively dispersed in distribution, belonging to the vanadium-containing resources which are difficult to process and utilize.
Because the high-carbon stone coal has higher carbon content, the carbon can cover the surfaces of stone coal mineral particles in the leaching process, and the adsorption capacity is extremely strong. Which is detrimental to the leaching of vanadium and seriously affects the leaching rate of vanadium and should therefore be removed beforehand. The main processes for treating high-carbon stone coal at present comprise: directly oxidizing, roasting, generating power, leaching tailings, reselecting or carrying out acid leaching or alkali leaching on the tailings after flotation and decarburization, and the like. The carbon content of the high-carbon stone coal ore is more than 10 percent, belongs to fuel with medium and low heat value, and is about one fifth of the heat value of the coal (Van Yan Qing, Wang Ling, Wang Hui, and the like)]Chinese resources comprehensive utilization, 2016, 34 (8)). When the stone coal is used for oxidizing and roasting power generation, sufficient heat required by power generation is not sufficiently provided, so that additional carbon matching is required. In addition, the process generates SO2And the treatment capacity of harmful gases such as CO and the like and large consumption of a large amount of acid or alkali and waste acid and waste alkali due to large amount of subsequent treatment slag. The direct oxidizing roasting power generation of high-carbon stone coal and the leaching process of tailings not only cause the waste of carbon resources, but also generate a large amount of greenhouse gases and waste acid and waste alkali to pollute the environment. When high-carbon stone coal is used for extracting vanadium, decarburization can be carried out by a physical ore dressing, namely a gravity separation or flotation method, so that the carbon resource is recovered while the vanadium grade is improved, and the subsequent vanadium leaching (Cheilong, Xianshenhong, Wangchun. high-carbon vanadium ore comprehensive recovery graphite test research is convenient [ J]Modern mining, 2007, 23(4): 35-37). However, when the high-carbon stone coal is pretreated by a flotation or gravity separation method, the loss of vanadium resources is caused, so that the recovery rate of vanadium is greatly reduced.
Therefore, the high-carbon vanadium-containing stone coal resource is treated by adopting a direct oxidation roasting power generation and tailing leaching process, and a vanadium-rich process of physical mineral separation pretreatment, and has the problems of a plurality of processes, cost and environmental protection.
Disclosure of Invention
The invention provides a method for green and efficient utilization of carbon resources and pre-enrichment of vanadium, which can convert carbon resources in high-carbon stone coal into clean energy in a green and efficient manner, and can obtain a vanadium-rich phase with high vanadium content and convenient separation. Compared with the prior art, the method can be used for green and high-efficiency treatment of high-carbon vanadium-containing stone coal resources, and has important significance for comprehensive utilization of the stone coal resources.
A method for green and efficient utilization of carbon in high-carbon vanadium-containing stone coal and pre-enrichment of vanadium mainly comprises the following steps: using high-carbon vanadium-containing coal mine as raw material, Fe2O3As an additive, MgO or Al2O3As modifier, the raw materials are crushed and fully mixed with additive and modifier to prepare pellets. After drying, gasifying by adopting a steam gasification process of carbon in high-carbon stone coal, stopping introducing steam after the gasification reaction is finished, and continuously raising the temperature to perform pre-enrichment of vanadium in the stone coal, wherein the roasting temperature is controlled to be 1000-1200 ℃. After the sintering, vanadium-containing enriched phase-vanadium iron spinel can be generated in the product. Because the vanadium iron spinel has magnetism, the vanadium iron spinel is crushed, ground and sieved and then is subjected to magnetic separation, and vanadium-containing concentrate with low impurity content and high vanadium grade can be obtained.
Further, in the steam gasification process of carbon in the high-carbon stone coal, after the high-carbon stone coal is pelletized and dried, steam or mixed gas of steam and argon is introduced at 800-900 ℃ to gasify carbon by using the steam, and the gasification time is 1-2 h. The steam gasification reaction of carbon can efficiently convert solid carbon resources in high-carbon stone coal into more green and environment-friendly CO and H with higher heat value2And the like. Compared with the conventional method for oxidizing, roasting and decarburizing the vanadium-containing stone coal, the method has the advantages that the carbon resource is more fully utilized, and the method is more energy-saving, environment-friendly and efficient.
Further, the additive Fe in the high-carbon stone coal2O3Reduced product of Fe3O4Not only can catalyze the water vapor gasification process of carbon, but also plays a role in enriching vanadium in the subsequent high-temperature roasting process. Wherein Fe is added when the mass of the added high-carbon vanadium-containing stone coal is x (g)2O3The mass is 0.05-0.15 x (g);
further, MgO or Al as a modifier in the high-carbon stone coal2O3The addition of the catalyst can effectively reduce the generation of low-melting-point substances and improve the integrity of roasted oreThe melting point of the body is reduced, thereby slowing down the high-temperature sintering phenomenon of the high-carbon stone coal mine and being more beneficial to the enrichment and the subsequent separation of vanadium. Wherein when the mass of the added high-carbon vanadium-containing stone coal is x (g), MgO or Al is added2O30.02 to 0.10x (g);
the high-carbon stone coal mainly contains SiO2、C、Al2O3And a small amount of K2O, MgO and V2O3. The high-carbon stone coal has high carbon content, and the vanadium existing in the mica ore has low grade, thus belonging to vanadium-containing resources which are difficult to process and utilize. The method adopts the idea of firstly utilizing the carbon resource and then enriching the vanadium resource to efficiently treat the high-carbon stone coal resource. Due to the introduction of steam and Fe2O3MgO or Al2O3The addition, at high temperature, mainly occurs the reaction shown below:
C(s)+H2O(g)＝CO(g)+H2(g) (1)
3Fe2O3(s)+C(s)＝2Fe3O4(s)+CO(g) (2)
Fe2O3(s)+C(s)＝2FeO(s)+CO(g) (3)
Fe2O3(s)+C(s)+2V2O3＝2FeV2O4(s)+CO(g) (4)
2FeO(s)+SiO2(s)＝2FeO·SiO2(s) (5)
3Al2O3(s)+2SiO2(s)＝3Al2O3·2SiO2(s) (6)
MgO(s)+SiO2(s)＝MgO·SiO2(s) (7)
the standard Gibbs free energies at different temperatures for each of the above reactions are shown in Table 1.
TABLE 1 Standard Gibbs free energy changes Δ for reactions (1) - (7) at different temperaturesrGθ
Figure BDA0002134243850000041
Mainly carrying out reverse reaction in the stage of high-carbon stone coal steam gasification and decarburizationThe formula (1) and (2). As is clear from FIG. 1, the (. DELTA.) of the reactions (1) and (2)rGθThe delta of reaction (2) at each temperature decreases with increasing temperaturerGθAre all smaller, indicating that the reaction is facile. Theoretically, under the condition of controlling the gasification temperature of 1073-1173K, the water vapor gasification reaction of carbon can be better carried out, and Fe can be better generated3O4And (4) phase(s). Additive Fe2O3The intermediate product not only can catalyze the water vapor gasification reaction of carbon, but also plays a role in subsequent vanadium enrichment.
And after the gasification is finished, raising the temperature to 1273-1473K, and performing vanadium pre-enrichment, wherein the main reactions in the stage are (3) - (7). As is clear from Table 1, reaction (4), i.e., vanadium enrichment reaction,. DELTA.rGθDecreases with increasing temperature and has a delta of 1273-1473KrGθMuch less than 0, so reaction (4) readily occurs under such conditions, i.e., it is demonstrated that vanadium resource enrichment is possible and feasible under such conditions.
In addition, at the roasting temperature of the pre-enriched vanadium, the reactions (3) and (5) can occur due to the existence of a large amount of carbon and quartz phases in the high-carbon stone coal, so that low-melting-point ferrosilicate can be generated, the sample is seriously sintered, and the enrichment and subsequent separation of the vanadium are not facilitated. Therefore, the modifier MgO or Al is added into the raw ore2O3So that the high-melting-point silicate is preferentially generated with the quartz phase, and the sintering phenomenon is slowed down. As can be seen from FIG. 2, at 800 to 1600K, the temperature increases, and the reaction (. DELTA.) of reaction (5)rGθContinuously increasing, and the Δ of reaction (6)rGθAre continuously decreasing. In addition, Delta of reaction (7)rGθIn this temperature range, much smaller than reactions (5), (6). Theoretically, under 1273-1473K, MgO & SiO2Most easily generated, 3Al when the temperature is higher than 1400K2O3·2SiO2Ratio of 2 FeO. SiO2It is easier to produce. Therefore, theoretically, the addition of the modifier can effectively reduce the generation of low-melting-point substances and improve the overall melting point of the roasted ore.
Compared with the prior art for treating high-carbon vanadium-containing stone coal, the method has the advantages that:
1. the method has the advantages of high resource utilization rate, energy conservation, environmental protection, high carbon gasification and vanadium enrichment efficiency and the like, can convert the carbon resource in the high-carbon stone coal into clean energy in an environment-friendly and efficient manner, and can obtain the vanadium-rich concentrate with high vanadium grade.
2. After pelletizing and drying the high-carbon stone coal, introducing mixed gas of water vapor and argon at 800-900 ℃ and gasifying carbon by using the water vapor, wherein the gasification time is 1-2 h. The steam gasification of carbon can efficiently convert the solid carbon resource in the high-carbon stone coal into CO and H with higher heat value and more environmental protection2Clean energy sources are used, and compared with the conventional method for oxidizing, roasting and decarburizing the vanadium-containing stone coal, the carbon resource is more fully utilized, and the method is more energy-saving, green, environment-friendly and efficient;
3. additive Fe in high-carbon stone coal2O3Intermediate product of Fe3O4The additive not only can catalyze the water vapor gasification process of carbon, but also plays a role in enriching vanadium in the subsequent high-temperature roasting process, is cheaper and easily obtained compared with other additives for treating the stone coal mine, and is green and environment-friendly;
4. modifier MgO or Al added in high-carbon stone coal2O3The generation of low-melting-point substances is effectively reduced, the high-temperature sintering phenomenon of the high-carbon stone coal mine can be greatly slowed down, and the sintering temperature is increased, so that the enrichment and subsequent separation of vanadium are facilitated; the roasting pre-enrichment process of vanadium resource in high carbon stone coal has roasting temperature controlled in 1000-1200 deg.c, and after roasting, vanadium-rich phase-ferrovanadium spinel may be produced in the product. Because the vanadium iron spinel has magnetism, the vanadium iron spinel is crushed, ground and sieved and then is subjected to magnetic separation, and vanadium-containing concentrate with low impurity content and high vanadium grade can be obtained.
Drawings
FIG. 1 shows the values of. DELTA.of reactions (1) to (2)rGθ-T-diagram, which shows that the gasification reaction of water vapor and carbon can be well performed in the range of 1000-1600K; and in the range of 800-1600K, Fe3O4The phase is easy to generate, can catalyze the water vapor gasification process of carbon, and plays a role in enriching vanadium in the subsequent high-temperature roasting process.
FIG. 2 shows the values of. DELTA.of reactions (5) to (7)rGθ-T diagram illustrating the thermodynamics of MgO or Al2O3The addition of the modifier can effectively reduce the generation of low-melting-point substances and improve the overall melting point of the roasted ore.
FIG. 3 is a comparison of XRD results of a magnetic separation concentrate sample after reaction of a raw ore sample and 1473K, which shows that after high-carbon vanadium-containing stone coal is subjected to carbon steam gasification and high-temperature vanadium pre-enrichment, a ferrovanadium spinel phase which is convenient to separate is generated in the sample.
FIG. 4a is a graph of a back-scattered analysis of a concentrate sample obtained by magnetic separation at a calcination temperature of 1473K (1200 ℃); figure 4b is the EDS dotting analysis result. According to the analysis result, the enriched phases with the compositions of Fe, V and O are indeed formed in the roasted sample, and the vanadium grade (calculated by metal vanadium) can reach 15%. This indicates that the effective enrichment of vanadium does occur under the roasting condition, and magnetic ferrovanadium spinel phase Fe is generated3-xVxO4。
Detailed Description
The present invention will be further explained with reference to specific examples in order to further understand and verify the present invention. In addition, the present invention is not limited to the following examples. All such modifications made in accordance with the spirit of the present invention are intended to be included within the scope of the present invention.
The raw material adopted in the experiment is high-carbon vanadium-containing stone coal raw ore in a certain place of south-Henan Yang. The ore is complex, contains a large amount of quartz and silicate minerals accounting for 61.37%, has a carbon content of 12.7%, mainly contains vanadium in mica minerals, and has a low vanadium content of about 0.27%, so the ore is a typical refractory high-carbon vanadium-containing stone coal. Crushing, grinding and sieving raw ore, and mixing with a certain amount of Fe2O3And MgO or Al2O3The mixture is fully and evenly mixed to be made into pellets, and the experiment is carried out after the pellets are dried. Wherein Fe is added when the mass of the added high-carbon vanadium-containing stone coal is x (g)2O3MgO or Al with the mass of 0.05-0.15 x (g) is added2O3Is 0.02 to 0.10x (g).
The invention adds Fe into raw ore2O3So that it firstly reacts with carbon in stone coal at a certain temp. and then converts carbon into CO and H at 800-900 deg.C after introducing steam2And (2) when clean energy is used, namely, the reaction shown in the formula (1) is mainly carried out, in the gasification experimental process, water vapor is brought into the reaction furnace by using argon, and the flow of the water vapor can be controlled by adjusting the flow of the argon. When the water vapor flow is constant, the gasification temperature is respectively controlled to be 800 ℃, 850 ℃ and 900 ℃, and the gasification time is respectively controlled to be 1h, 1.5h and 2 h. According to the experimental result, when the gasification temperature is 900 ℃ and the gasification time is 1.5h and 2h respectively, the conversion rate of the carbon is respectively as high as 92.4 percent and 99.6 percent.
It is worth mentioning that the additive Fe2O3Intermediate product Fe3O4Has catalytic action on the carbon steam gasification process, and can greatly accelerate the gasification process. In order to verify the catalytic effect, the following experiment was carried out under the conditions of the gasification temperature of 900 ℃ and the gasification time of 1.5h, and Fe was added to the sample 12O3Sample 2 without Fe2O3. After single variable experiments, the carbon conversion was 92.4% and 66% in samples 1 and 2, respectively. Thus, the experimental results show that the additive Fe2O3Reduction product Fe3O4Has obvious catalytic action on the steam gasification process.
And after the gasification is finished, stopping introducing water vapor and continuously raising the temperature to carry out roasting pre-enrichment of the vanadium resource, wherein the roasting temperature is controlled at 1000 ℃, 1150 ℃ and 1200 ℃, the roasting time is 3h, and the reaction atmosphere is high-purity argon (99.999%). As can be seen from the reaction formula (4), the ferrovanadium spinel phase can be obtained in the roasted product, and vanadium-containing concentrate with low impurity content and high vanadium grade is separated by magnetic separation, wherein the vanadium grade can reach 11.33%, and the vanadium grade is improved by 24 times compared with that of the original ore.
And (3) carrying out XRD (x-ray diffractometer), SEM-EDS (scanning electron microscope spectrometer) and ICP (inductively coupled plasma spectrometer) detection on the magnetic separation concentrate and the raw ore sample after roasting at the temperature of 1473K (1200 ℃). FIG. 3 is an XRD comparison diagram of raw ore and magnetic concentrate, and FIG. 4 is an SEM-EDS diagram of magnetic concentrate.
As can be seen from FIG. 3, by comparing the XRD results of 1473K (1200 ℃ C.) with those of the original sample and calibrating the newly formed substance, it was found that the vanadium iron spinel (Fe) is mainly contained in the newly formed substance3-xVxO4) and contains a small amount of Fe. In addition, as can be seen from the results of the scanning electron microscope of FIG. 4, Fe was indeed found in the magnetic concentrate3-xVxO4A phase. In order to explain the enrichment effect more visually, the ICP is used for analyzing vanadium elements of the magnetic concentrate and the raw ore, so that the vanadium content of the raw ore is about 0.27%, the vanadium content of the magnetic concentrate is 6.35%, the vanadium content is improved by more than 20 times, and the pre-enrichment effect is obvious.

Claims (1)

1. A method for green and efficient utilization of carbon in high-carbon vanadium-containing stone coal and pre-enrichment of vanadium mainly comprises the following steps: using high-carbon vanadium-containing coal mine as raw material, Fe2O3As an additive, MgO or Al2O3As a modifier, crushing the raw materials, fully mixing the crushed raw materials with the additive and the modifier, and then preparing pellets; after drying, gasifying by adopting a steam gasification process of carbon in high-carbon stone coal, stopping introducing steam after the gasification reaction is finished, and continuously raising the temperature to perform pre-enrichment of vanadium in the stone coal, wherein the roasting temperature is controlled to be 1000-1200 ℃; after the baking and sintering, vanadium-containing enriched phase-vanadium iron spinel can be generated in the product; because the vanadium iron spinel has magnetism, the vanadium iron spinel is crushed, ground and sieved and then is subjected to magnetic separation, and vanadium-containing concentrate with low impurity content and high vanadium grade can be obtained;
the steam gasification process of the carbon in the high-carbon stone coal comprises the steps of pelletizing and drying the high-carbon stone coal, introducing steam or mixed gas of the steam and argon at 800-900 ℃, and gasifying the carbon by using the steam, wherein the gasification time is 1-2 h;
when the mass of the added high-carbon vanadium-containing stone coal is x (g), Fe is added2O3The mass is 0.05-0.15 x (g);
when the mass of the added high-carbon vanadium-containing stone coal is x (g), MgO or Al is added2O3Is 0.02 to 0.10x (g).
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GB816609A (en) * 1956-05-01 1959-07-15 United Steel Companies Ltd Improvements relating to the recovery of vanadium from slag
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CN106756117A (en) * 2016-12-14 2017-05-31 安徽工业大学 A kind of method that Rock coal containing alum and v-bearing steel slag combine vanadium enrichment
CN107267701A (en) * 2017-07-24 2017-10-20 江苏省冶金设计院有限公司 A kind of pyrolysis of coal, pyrolysis gas heating and the system and method for schreyerite reduction coupling
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