CN101397150A - A method for extracting vanadium pentoxide from vanadium-containing converter steel slag - Google Patents
A method for extracting vanadium pentoxide from vanadium-containing converter steel slag Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 57
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 42
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910000831 Steel Inorganic materials 0.000 title claims description 44
- 239000010959 steel Substances 0.000 title claims description 44
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000002699 waste material Substances 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 30
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 16
- 238000002386 leaching Methods 0.000 claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 29
- 235000010215 titanium dioxide Nutrition 0.000 claims description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 8
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
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- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
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- 239000007800 oxidant agent Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000011469 building brick Substances 0.000 claims description 2
- 238000010979 pH adjustment Methods 0.000 claims description 2
- 239000012066 reaction slurry Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000000243 solution Substances 0.000 description 21
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000003350 kerosene Substances 0.000 description 4
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 description 1
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- CZSABVBCTRZESY-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].OS(O)(=O)=O Chemical compound [O-2].[O-2].[Ti+4].OS(O)(=O)=O CZSABVBCTRZESY-UHFFFAOYSA-N 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种从含钒转炉钢渣中提取五氧化二钒的方法，本发明采用的技术方案主要是用钛白废酸提取转炉钢渣。该工艺的最大特点是以废治废，节省了钛白废酸的治理成本；用钛白废酸浸出转炉钢渣提取其中的钒，大大降低了转炉钢渣提钒的成本，并可使钛白废酸得到回收利用。用该工艺提取转炉钢渣中的钒，钒浸出率可达80％以上。
The present invention relates to a method for extracting vanadium pentoxide from vanadium-containing converter slag. The technical solution adopted by the present invention is mainly to extract converter slag with titanium dioxide waste acid. The biggest feature of the process is to treat waste with waste, saving the cost of treating titanium dioxide waste acid; using titanium dioxide waste acid to leach converter slag to extract vanadium therein greatly reduces the cost of extracting vanadium from converter slag, and can recycle titanium dioxide waste acid. Using the process to extract vanadium from converter slag, the vanadium leaching rate can reach more than 80%.
Description
技术领域 technical field
本发明涉及一种从含钒转炉钢渣中提取五氧化二钒的工艺。The invention relates to a process for extracting vanadium pentoxide from vanadium-containing converter steel slag.
背景技术 Background technique
目前，在钢铁冶炼过程中产生了大量的含钒转炉钢渣，由于其中的氧化钙含量高，钒含量低，采用传统的钠化焙烧—水浸提钒工艺，难以有效地将其中的钒提出；而如果采用硫酸浸出工艺，则硫酸消耗大，经济上不可行，因此未对该工艺进行实际应用何优化深入研究。也就是说目前尚未有经济、合理的工艺来提取转炉钢渣中的钒，因此，大量的转炉钢渣中的钒没有得到有效地回收，处于废弃状态，污染环境。At present, a large amount of vanadium-containing converter steel slag is produced in the iron and steel smelting process. Due to the high calcium oxide content and low vanadium content in it, it is difficult to effectively extract the vanadium from it by using the traditional sodium roasting-water leaching vanadium extraction process; However, if the sulfuric acid leaching process is adopted, the consumption of sulfuric acid is large, and it is not economically feasible, so no in-depth research on the actual application and optimization of this process has been carried out. That is to say, there is no economical and reasonable process to extract the vanadium in the converter steel slag. Therefore, a large amount of vanadium in the converter steel slag has not been effectively recovered, and it is in a waste state and pollutes the environment.
目前以含钒石煤为原料的生产工艺中，有使用P204萃取—硫酸反萃—氧化—沉钒的工艺，但该工艺适用于溶液中杂质种类和含量较少的情况，含钒转炉钢渣中含大量Fe2+、Fe3+、Mg2+、Al3+、Mn2+、SO4 2-等杂质，同时还含有与钒含量相当的TiO2+等，成分相当复杂，采用现有的萃取—反萃工艺难以将钒与其它杂质分离。At present, in the production process using vanadium-containing stone coal as raw material, there is a process of using P204 extraction-sulfuric acid stripping-oxidation-precipitation of vanadium, but this process is suitable for the situation where the type and content of impurities in the solution are small, and the vanadium-containing converter steel slag Contains a large amount of impurities such as Fe 2+ , Fe 3+ , Mg 2+ , Al 3+ , Mn 2+ , SO 4 2-, etc., and also contains TiO 2+ with a content equivalent to that of vanadium. The composition is quite complex, and the existing The extraction-stripping process is difficult to separate vanadium from other impurities.
另一方面，国内钛白粉生产以硫酸法钛白工艺为主，每生产一吨钛白粉会产生200g/l～300g/l的废硫酸7t，本领域一般称为钛白废酸，目前多数钛白废酸以石灰中和法简单处理了事，甚至不加处理直接排入江河，严重污染环境。On the other hand, domestic titanium dioxide production is mainly based on the sulfuric acid titanium dioxide process. Every ton of titanium dioxide produced will produce 200g/l-300g/l waste sulfuric acid 7t, which is generally called titanium dioxide waste acid in this field. At present, most titanium dioxide The white waste acid is simply disposed of by lime neutralization, and even discharged directly into rivers without treatment, seriously polluting the environment.
因此，本领域急需开发一种能同时高效处理上述两种废弃材料的方法。Therefore, there is an urgent need in the art to develop a method that can efficiently process the above two waste materials simultaneously.
发明内容 Contents of the invention
本发明针对转炉钢渣氧化钙含量高，采用硫酸浸出工艺耗酸量大的特点，提出了一种以废治废的工艺，即用钛白废酸浸出转炉钢渣，这不仅节省了钛白废酸的治理成本，也使转炉钢渣硫酸浸出工艺经济上可行。该工艺有工艺流程短、产业化设备简单等特点。Aiming at the high content of calcium oxide in converter steel slag and the large acid consumption of the sulfuric acid leaching process, the present invention proposes a process of treating waste with waste, that is, leaching converter steel slag with waste titanium white acid, which not only saves waste titanium white acid The cost of treatment also makes the converter steel slag sulfuric acid leaching process economically feasible. The process has the characteristics of short process flow and simple industrial equipment.
结合本发明的目的，通过以下技术解决方案来实现：In conjunction with the purpose of the present invention, it is achieved through the following technical solutions:
一种从含钒转炉钢渣中提取五氧化二钒的方法，该方法包括以下步骤：A method for extracting vanadium pentoxide from vanadium-containing converter steel slag, the method comprises the following steps:
a、将转炉钢渣破碎；a. Break the converter steel slag;
b、将破碎的转炉钢渣加入到搅拌状态下的钛白废酸中反应；b. Add the broken converter steel slag to the titanium dioxide waste acid in the stirred state to react;
c、将酸浸反应浆料固液分离，固液分离后的固体用于制造建筑砖材；c. The acid leaching reaction slurry is separated from solid to liquid, and the solid after solid-liquid separation is used to manufacture building bricks;
d、除去步骤c中固液分离后的溶液中的三价铁，然后调节溶液的pH＝1.5～3.0；d, remove the ferric iron in the solution after solid-liquid separation in step c, then adjust the pH of the solution=1.5～3.0;
e、对调节pH后的溶液固液分离；e. Solid-liquid separation of the solution after pH adjustment;
f、对步骤e固液分离后得到的溶液进行萃取—反萃；f, the solution obtained after the solid-liquid separation of step e is extracted-back-extracted;
g、按理论量的1.3～1.6倍加入氧化剂将反萃液中的四价钒氧化为五价，沉钒，即得。g. Add an oxidizing agent according to 1.3-1.6 times of the theoretical amount to oxidize the tetravalent vanadium in the stripping solution to pentavalent, and precipitate the vanadium to obtain the product.
其中，上述方法步骤a中转炉钢渣破碎的大小为0.3mm以下。Wherein, the broken size of the converter steel slag in step a of the above method is less than 0.3 mm.
其中，上述方法步骤b中所述钛白废酸的浓度为200～300g/l。Wherein, the concentration of the titanium dioxide waste acid in step b of the above method is 200-300 g/l.
其中，上述方法步骤b中将转炉钢渣加入到钛白废酸中时，体系的搅拌速度控制在300～600rpm。反应体系的温度为常温即可。Wherein, when the converter steel slag is added to the titanium white waste acid in step b of the above method, the stirring speed of the system is controlled at 300-600 rpm. The temperature of the reaction system may be normal temperature.
其中，上述方法步骤b中钛白废酸与转炉钢渣反应时，转炉钢渣加入量为控制反应终点溶液pH＝0.5～2.5。Wherein, when the spent titanium dioxide acid reacts with the converter steel slag in step b of the above method, the amount of converter steel slag added is to control the pH of the solution at the end of the reaction to be 0.5-2.5.
其中，上述方法步骤b中钛白废酸与转炉钢渣的反应时间为40min～120min。Wherein, the reaction time between the titanium dioxide waste acid and the converter steel slag in step b of the above method is 40 minutes to 120 minutes.
其中，上述方法步骤d中溶液除三价铁的方法是添加铁粉还原。本发明中所述的除三价铁是指将三价铁还原。Wherein, the method for removing ferric iron from the solution in step d of the above method is to add iron powder for reduction. The removal of ferric iron in the present invention refers to the reduction of ferric iron.
其中，上述方法步骤d中用来调节溶液pH值的碱性物质为氢氧化钠、氢氧化钾、石灰乳、碳酸钠中的至少一种。Wherein, the alkaline substance used to adjust the pH value of the solution in step d of the above method is at least one of sodium hydroxide, potassium hydroxide, milk of lime, and sodium carbonate.
其中，上述方法步骤f中萃取所用的萃取剂为P204∶溶剂油∶TBP体积比为10～20∶75～88∶2～5的混合物。P204即为二(2乙基己基)磷酸、TBP为磷酸三丁酯。其中的溶剂油优选为260号溶剂油(又称磺化煤油)或普通煤油。Wherein, the extraction agent used in the extraction in step f of the above method is a mixture of P204: solvent oil: TBP volume ratio of 10-20: 75-88: 2-5. P204 is two (2 ethylhexyl) phosphoric acid, TBP is tributyl phosphate. The solvent oil wherein is preferably No. 260 solvent oil (also known as sulfonated kerosene) or common kerosene.
进一步的，上述方法步骤f中反萃所用的反萃剂为1.2～1.8mol/L的硫酸或盐酸。优选为使用1.5mol/L的硫酸或盐酸。Further, the stripping agent used in the stripping step f of the above method is 1.2-1.8 mol/L sulfuric acid or hydrochloric acid. Preferably, 1.5 mol/L sulfuric acid or hydrochloric acid is used.
其中，上述方法步骤g中的氧化剂可使用氯酸钠、过氧化氢、次氯酸钠或过硫酸铵中的至少一种。Wherein, at least one of sodium chlorate, hydrogen peroxide, sodium hypochlorite or ammonium persulfate can be used as the oxidizing agent in step g of the above method.
本发明针对转炉钢渣中氧化钙含量高，且采用硫酸浸出工艺耗酸量大的特点，采用以废治废的思想，即用主要用钛白废酸浸出转炉钢渣。其中对具体的工艺步骤及参数以及萃取剂等原料进行了优化，达到了预期的效果。本发明方法不仅节省了钛白废酸的治理成本，也使转炉钢渣的治理成本大为降低，既回收了有用的品位在98％以上的五氧化二钒，也大大降低了污染物的排放量，所产生的经济效益可弥补三废处理增加的相应成本。本发明方法工艺流程短、反应条件温和、设备简单，具有很好的应用前景。Aiming at the high content of calcium oxide in the converter steel slag and the large acid consumption of the sulfuric acid leaching process, the invention adopts the idea of treating waste with waste, that is, the converter steel slag is leached mainly with titanium white waste acid. Among them, the specific process steps and parameters, as well as raw materials such as extractant were optimized, and the expected effect was achieved. The method of the invention not only saves the treatment cost of titanium white waste acid, but also greatly reduces the treatment cost of converter steel slag, not only recovers the useful vanadium pentoxide with a grade of more than 98%, but also greatly reduces the discharge of pollutants , the resulting economic benefits can make up for the corresponding increase in the cost of the three wastes treatment. The method of the invention has short process flow, mild reaction conditions, simple equipment and good application prospect.
附图说明 Description of drawings
图1表示的是本发明方法的简要流程What Fig. 1 represented is the brief flow process of the inventive method
具体实施方式 Detailed ways
下面结合实施例对本发明作进一步地说明，其中所用的P204、TBP和磺化煤油均为普通市售工业级产品。The present invention will be further described below in conjunction with the examples, wherein the P204, TBP and sulfonated kerosene used are all commercially available industrial grade products.
实施例一Embodiment one
取粉碎到-60目，全钒(TV)含量为0.707％的转炉钢渣50g，加入到250ml硫酸浓度为208g/l的钛白废酸中，常温搅拌40min，过滤、洗涤后将残渣烘干。残渣重52.1g，TV含量为0.120％，钒浸出率82.31％。浸出液体积270ml，TV浓度为1.13g/l。Take 50 g of converter steel slag crushed to -60 mesh, with a total vanadium (TV) content of 0.707%, add it to 250 ml of titanium white waste acid with a sulfuric acid concentration of 208 g/l, stir at room temperature for 40 min, filter, wash and dry the residue. The residue weighs 52.1g, the TV content is 0.120%, and the vanadium leaching rate is 82.31%. The volume of the leach solution is 270ml, and the TV concentration is 1.13g/l.
实施例二Embodiment two
取粉碎到-60目，TV含量为0.707％的转炉钢渣50g，加入到200ml硫酸浓度为278g/l的钛白废酸中，常温搅拌120min，过滤、洗涤后将残渣烘干。残渣重52.8g，TV含量为0.111％，钒浸出率83.47％。浸出液体积235ml，TV浓度为1.29g/l。Take 50g of converter steel slag crushed to -60 mesh and TV content of 0.707%, add it to 200ml of titanium white waste acid with a sulfuric acid concentration of 278g/l, stir at room temperature for 120min, filter, wash and dry the residue. The residue weighs 52.8g, the TV content is 0.111%, and the vanadium leaching rate is 83.47%. The volume of the leachate was 235ml, and the TV concentration was 1.29g/l.
实例三Example three
按实施例一、二的具体方法重复处理多次，将各次所得的含钒溶液混合。所得混合液的体积为5300ml，主要成分为：TV＝1.32g/l、Fe3+＝9.75g/l、Ca2+＝0.559g/l、Mg2+＝19.53g/l、Fe2+＝53.50g/l、Al3+＝3.75g/l、SiO2＝0.172g/l、Ti＝4.01g/l、Mn2+＝2.68g/l、P＝0.688g/l。Repeat the treatment several times according to the specific method of embodiment 1 and 2, and mix the vanadium-containing solutions obtained each time. The volume of the obtained mixed solution is 5300ml, and the main components are: TV = 1.32g/l, Fe 3+ =9.75g/l, Ca 2+ =0.559g/l, Mg 2+ =19.53g/l, Fe 2+ = 53.50 g/l, Al 3+ =3.75 g/l, SiO 2 =0.172 g/l, Ti=4.01 g/l, Mn 2+ =2.68 g/l, P=0.688 g/l.
实施例四Embodiment four
取实施例三中多次转炉钢渣与钛白废酸反应所得的含钒溶液2000ml，其主要成分为：TV＝1.32g/l、Fe3+＝9.75g/l、Ca2+＝0.559g/l、Mg2+＝19.53g/l、Fe2+＝53.50g/l、Al3+＝3.75g/l、SiO2＝0.172g/l、Ti＝4.01g/l、Mn2+＝2.68g/l、P＝0.688g/l。向该溶液加入铁粉11.7g，常温搅拌4小时，加入石灰乳调节溶液pH＝2.32后过滤，滤液用由15％P204+5％TBP+80％磺化煤油组成的萃取剂萃取，然后用1.5mol/l的硫酸反萃，反萃液加入氯酸钠氧化后沉钒，得到多钒酸铵4.61g，进一步在600～800℃下加热熔化，得到片状五氧化二钒3.96g，其品位为98.7％。Get 2000ml of the vanadium-containing solution obtained from the reaction of converter steel slag and titanium dioxide waste acid many times in Example 3, its main components are: TV=1.32g/l, Fe 3+ =9.75g/l, Ca 2+ =0.559g/l l. Mg 2+ = 19.53g/l, Fe 2+ = 53.50g/l, Al 3+ = 3.75g/l, SiO 2 = 0.172g/l, Ti = 4.01g/l, Mn 2+ = 2.68g /l, P=0.688g/l. Add 11.7g of iron powder to the solution, stir at room temperature for 4 hours, add milk of lime to adjust the pH of the solution to 2.32, and then filter. mol/l sulfuric acid stripping, adding sodium chlorate to the stripping solution to oxidize and then precipitate vanadium to obtain 4.61g of ammonium polyvanadate, which is further heated and melted at 600-800°C to obtain 3.96g of flake vanadium pentoxide. was 98.7%.
实例五Example five
取实施例三中制备的转炉钢渣与钛白废酸反应所得的含钒溶液2000ml，其主要成分为：TV＝1.32g/l、Fe3+＝9.75g/l、Ca2+＝0.559g/l、Mg2+＝19.53g/l、Fe2+＝53.50g/l、Al3+＝3.75g/l、SiO2＝0.172g/l、Ti＝4.01g/l、Mn2+=2.68g/l、P＝0.688g/l。将该溶液煮沸腾，用碳酸钠调节溶液pH＝1.65，搅拌条件下加入硫酸钠12.36g，反应2小时，加入石灰乳调节溶液pH＝2.50后过滤，滤液用由15％P204+5％TBP+80％磺化煤油组成的萃取剂萃取，然后用1.5mol/l的硫酸反萃，反萃液加入氯酸钠氧化后沉钒，得到多钒酸铵4.69g，进一步在600～800℃下加热熔化得到片状五氧化二钒4.10g，其品位为98.5％。Get the vanadium-containing solution 2000ml that the converter steel slag that prepares in the embodiment three reacts with titanium white waste acid to gain, its main component is: TV=1.32g/l, Fe 3+ =9.75g/l, Ca 2+ =0.559g/l l. Mg 2+ = 19.53g/l, Fe 2+ = 53.50g/l, Al 3+ = 3.75g/l, SiO 2 = 0.172g/l, Ti = 4.01g/l, Mn 2+ = 2.68g /l, P=0.688g/l. Boil the solution, adjust the pH of the solution to 1.65 with sodium carbonate, add 12.36 g of sodium sulfate under stirring conditions, react for 2 hours, add milk of lime to adjust the pH of the solution to 2.50, and then filter. The filtrate is made of 15% P204+5%TBP+ Extract with an extractant composed of 80% sulfonated kerosene, then back-extract with 1.5mol/l sulfuric acid, add sodium chlorate to the back-extraction solution to oxidize and precipitate vanadium to obtain 4.69g of ammonium polyvanadate, and further heat at 600-800°C Melted to obtain 4.10 g of flaky vanadium pentoxide with a grade of 98.5%.
本发明针对转炉钢渣氧化钙含量高，采用现有硫酸浸出工艺耗酸量大的特点，采用以废治废的思想，即主要用钛白废酸浸出转炉钢渣，并对其中具体的工艺步骤及参数以及萃取剂等原料进行了优化，使钒浸出率可达80％以上，五氧化二钒品位在98以上。本发明方法既回收了有用的五氧化二钒，也大大降低了污染物的排放量。本发明方法工艺流程短、反应条件温和、设备简单，具有很好的应用前景。Aiming at the high content of calcium oxide in converter steel slag, the present invention adopts the characteristics of large acid consumption in the existing sulfuric acid leaching process, adopts the idea of treating waste with waste, that is, mainly uses titanium white waste acid to leach converter steel slag, and discusses the specific process steps and The parameters and raw materials such as extraction agent are optimized, so that the vanadium leaching rate can reach more than 80%, and the grade of vanadium pentoxide is more than 98. The method of the invention not only recovers the useful vanadium pentoxide, but also greatly reduces the emission of pollutants. The method of the invention has short process flow, mild reaction conditions, simple equipment and good application prospect.
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| CN102560115A (en) * | 2012-02-07 | 2012-07-11 | 九江佰盾钒技术贸易有限公司 | Method for extracting vanadium from stone coal vanadium mine extraction |
| CN103555941A (en) * | 2013-11-14 | 2014-02-05 | 武汉科技大学 | Method for preparing extraction stock solution through stone coal vanadium extraction |
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| CN104017999A (en) * | 2014-06-25 | 2014-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method for converter vanadium slag |
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| CN109609775B (en) * | 2018-12-31 | 2020-08-07 | 南京格洛特环境工程股份有限公司 | Resource comprehensive utilization method of steel slag |
| CN112176208A (en) * | 2020-10-29 | 2021-01-05 | 攀枝花市山青钒业有限公司 | Method for co-extracting vanadium and scandium by using titanium white waste acid and vanadium-containing high-calcium high-phosphorus slag |
| CN112176208B (en) * | 2020-10-29 | 2021-10-26 | 攀枝花市山青钒业有限公司 | Method for co-extracting vanadium and scandium by using titanium white waste acid and vanadium-containing high-calcium high-phosphorus slag |
| CN112830694A (en) * | 2021-01-15 | 2021-05-25 | 攀枝花恒通钛业有限公司 | Method for comprehensively treating vanadium-containing furnace slag and titanium dioxide waste acid |
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