CN106006734A - Method of using vanadium-containing solution for preparing vanadium trioxide - Google Patents
Method of using vanadium-containing solution for preparing vanadium trioxide Download PDFInfo
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 38
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 title abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000012065 filter cake Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 4
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 4
- 229910021541 Vanadium(III) oxide Inorganic materials 0.000 claims 9
- -1 hydrogen ions Chemical class 0.000 abstract description 2
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 20
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical group [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 150000003863 ammonium salts Chemical class 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 1
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 1
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- KFAFTZQGYMGWLU-UHFFFAOYSA-N oxo(oxovanadiooxy)vanadium Chemical compound O=[V]O[V]=O KFAFTZQGYMGWLU-UHFFFAOYSA-N 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
技术领域technical field
本发明属于有色金属冶金领域，尤其涉及一种利用含钒溶液制备三氧化二钒的方法。The invention belongs to the field of nonferrous metal metallurgy, and in particular relates to a method for preparing vanadium trioxide from a vanadium-containing solution.
背景技术Background technique
三氧化二钒是钒的重要化合物，在冶金、电子、化工等行业有着重要的应用。三氧化二钒可用于制取钒铁和金属钒粉，也可作为制取碳化钒和氮化钒的原料；由于具有优异的光、电、磁性质，三氧化二钒在电、磁、光开关及气敏传感器、存储材料、电阻材料等多种领域都具有广泛的应用前景。Vanadium trioxide is an important compound of vanadium, which has important applications in metallurgy, electronics, chemical industry and other industries. Vanadium trioxide can be used to produce ferrovanadium and metal vanadium powder, and can also be used as a raw material for producing vanadium carbide and vanadium nitride; due to its excellent optical, electrical and magnetic properties, vanadium trioxide Switches and gas sensors, storage materials, resistance materials and other fields have broad application prospects.
目前，制备三氧化二钒的方法主要有两种：一种是不外加还原剂的偏钒酸铵或多聚钒酸铵热分解裂解法，如中国专利200610020405.7，利用加热偏钒酸铵时释放出的氨的热裂解产生的初生氢来还原偏钒酸铵，这种方法不采用外加还原气，虽然可以降低部分成本，但是原料分解出的氨气裂解不完全，不仅导致还原气氛不够，而且没有裂解的氨气的排除会造成环境污染。At present, there are two main methods for preparing vanadium trioxide: one is ammonium metavanadate or ammonium polyvanadate thermal decomposition cracking method without adding a reducing agent, such as Chinese patent 200610020405.7, which releases when the ammonium metavanadate is heated. The ammonium metavanadate is reduced by the primary hydrogen produced by the thermal cracking of the ammonia produced. This method does not use additional reducing gas. Although it can reduce part of the cost, the ammonia gas decomposed from the raw material is not completely cracked, which not only leads to insufficient reducing atmosphere, but also reduces the cost. The removal of ammonia without cracking will cause environmental pollution.
另一种制备三氧化二钒的方法是外加还原剂的直接高温还原法，多以C、NH3、H2、CH4、CO或工业煤气等为还原剂，热还原偏钒酸铵、多聚钒酸铵、五氧化二钒等高价钒化合物而获得三氧化二钒，此种方法也是目前广泛应用的制备三氧化二钒的方法。中国专利CN1118765A公开了一种三氧化二钒的生产方法，该方法以工业煤气为还原气体，在回转窑中对偏钒酸铵或五氧化二钒进行还原热解反应，获得三氧化二钒。该方法的缺点是：还原温度为900℃以上，能耗高，生产成本高；中国专利CN200610020405.7公开了一种生产粉体三氧化二钒的方法。其方法是将粉体钒酸铵或五氧化二钒作为炉料加入到外加热流态化炉炉管中，使炉管的填充率达到10％～55％，通入工业煤气，加热至600～650℃，保温还原以制备三氧化二钒。该技术方案的缺点是：还原温度高，能耗高，工业煤气用量大，生产工艺复杂，生产成本高。Another way to prepare vanadium trioxide is the direct high-temperature reduction method with an external reducing agent, mostly using C, NH 3 , H 2 , CH 4 , CO or industrial gas as the reducing agent, thermally reducing ammonium metavanadate, poly Vanadium trioxide is obtained from high-valent vanadium compounds such as ammonium polyvanadate and vanadium pentoxide. This method is also a widely used method for preparing vanadium trioxide. Chinese patent CN1118765A discloses a production method of vanadium trioxide. In the method, industrial gas is used as reducing gas, and ammonium metavanadate or vanadium pentoxide is reduced and pyrolyzed in a rotary kiln to obtain vanadium trioxide. The disadvantages of this method are: the reduction temperature is above 900°C, the energy consumption is high, and the production cost is high; Chinese patent CN200610020405.7 discloses a method for producing powdered vanadium trioxide. The method is to add powdered ammonium vanadate or vanadium pentoxide as charge into the furnace tube of the externally heated fluidized furnace, so that the filling rate of the furnace tube reaches 10% to 55%, and then feed industrial gas and heat to 600 to 650 ℃, heat preservation and reduction to prepare vanadium trioxide. The disadvantages of this technical solution are: high reduction temperature, high energy consumption, large amount of industrial gas consumption, complex production process and high production cost.
从已公开的资料可以看出，目前的三氧化二钒制备技术大都是以偏钒酸铵、多聚钒酸铵或五氧化二钒为原料，在一定的温度和还原气氛下反应所得，反应温度一般大于500℃，能耗高，生产成本高。偏钒酸铵、多聚钒酸铵大都是由提钒工业所得到的含钒溶液经铵盐沉淀所得；五氧化二钒为偏钒酸铵、多聚钒酸经热分解所得。因此，若以偏钒酸铵、多聚钒酸铵为原料制备三氧化二钒实则需要两步：(1)含钒溶液经铵盐沉淀制备偏钒酸铵、多聚钒酸铵，(2)以偏钒酸铵、多聚钒酸铵为原料在高温以及还原性气氛下制备三氧化二钒；若以五氧化二钒为原料制备三氧化二钒实则需要三步：(1)含钒溶液经铵盐沉淀制备偏钒酸铵、多聚钒酸铵，(2)偏钒酸铵、多聚钒酸铵经热分解制备五氧化二钒，(3)以五氧化二钒为原料在高温以及还原性气氛下制备三氧化二钒。可以看出，目前的三氧化二钒制备工艺较为复杂，复杂的制备工艺也造成生产成本的增加。同时，在铵盐沉淀制备偏钒酸铵、多聚钒酸铵的过程中会产生大量的氨氮废水，热分解偏钒酸铵、多聚钒酸铵制备五氧化二钒的过程会释放大量的氨气，这些废水和废气都会对环境造成严重的污染；另外，以偏钒酸铵或多聚钒酸铵为原料，在制备三氧化二钒的过程中会分解出大量的氨气，未反应的氨气释放到大气中同样会对环境造成污染。因此，现有的三氧化二钒制备工艺存在环境污染严重的问题。It can be seen from the published information that most of the current vanadium trioxide preparation technologies use ammonium metavanadate, ammonium polyvanadate or vanadium pentoxide as raw materials, which are obtained by reaction at a certain temperature and a reducing atmosphere. The temperature is generally higher than 500°C, the energy consumption is high, and the production cost is high. Ammonium metavanadate and ammonium polyvanadate are mostly obtained from the vanadium-containing solution obtained in the vanadium extraction industry through ammonium salt precipitation; vanadium pentoxide is obtained by thermal decomposition of ammonium metavanadate and polyvanadate. Therefore, if take ammonium metavanadate, ammonium polyvanadate as raw material to prepare divanadium trioxide actually need two steps: (1) vanadium-containing solution prepares ammonium metavanadate, ammonium polyvanadate through ammonium salt precipitation, (2 ) using ammonium metavanadate and ammonium polyvanadate as raw materials to prepare vanadium trioxide under high temperature and reducing atmosphere; if vanadium pentoxide is used as raw material to prepare vanadium trioxide, three steps are actually required: (1) vanadium-containing The solution is precipitated by ammonium salt to prepare ammonium metavanadate and ammonium polyvanadate, (2) ammonium metavanadate and ammonium polyvanadate are thermally decomposed to prepare vanadium pentoxide, (3) vanadium pentoxide is used as raw material in Preparation of vanadium trioxide under high temperature and reducing atmosphere. It can be seen that the current preparation process of vanadium trioxide is relatively complicated, and the complicated preparation process also causes an increase in production cost. Simultaneously, a large amount of ammonia nitrogen waste water can be produced in the process of preparing ammonium metavanadate and ammonium polyvanadate by ammonium salt precipitation, and the process of thermally decomposing ammonium metavanadate and ammonium polyvanadate to prepare vanadium pentoxide will release a large amount of Ammonia, these waste water and waste gas all can cause serious pollution to environment; In addition, use ammonium metavanadate or ammonium polyvanadate as raw material, can decompose a large amount of ammonia in the process of preparing vanadium trioxide, unreacted The release of ammonia gas into the atmosphere will also pollute the environment. Therefore, the existing vanadium trioxide preparation process has the problem of serious environmental pollution.
综上所述，现有的三氧化二钒制备工艺存在工艺复杂、环境污染严重、生产成本高的劣势。目前，急需寻求一种工艺简单、环境友好、生产成本低的三氧化二钒制备工艺。To sum up, the existing vanadium trioxide preparation process has the disadvantages of complicated process, serious environmental pollution and high production cost. At present, there is an urgent need to find a vanadium trioxide preparation process with simple process, environmental friendliness and low production cost.
发明内容Contents of the invention
本发明旨在解决上述三氧化二钒制备工艺的缺陷，目的是提供一种工艺简单、环境友好、生产成本低的三氧化二钒制备方法。The present invention aims to solve the defects of the above-mentioned vanadium trioxide preparation process, and aims to provide a vanadium trioxide preparation method with simple process, environment-friendly and low production cost.
为实现上述目的，本发明采用的技术方案是：利用含钒溶液制备三氧化二钒的方法，其步骤如下：In order to achieve the above object, the technical scheme adopted in the present invention is: utilize the method for preparing vanadium trioxide by vanadium-containing solution, and its steps are as follows:
采用氢气与钒浓度大于6g/L、氢离子浓度为10-4～10-14mol/L的含钒溶液在高温高压反应装置中搅拌反应1小时以上，所述的含钒溶液中的钒以五价态的形式存在，得到三氧化二钒水浆，其中，反应温度为50～300℃，氢气分压大于1MPa；Using hydrogen gas and a vanadium-containing solution with a vanadium concentration greater than 6g/L and a hydrogen ion concentration of 10 -4 to 10 -14 mol/L to stir and react in a high-temperature and high-pressure reaction device for more than 1 hour, the vanadium in the vanadium-containing solution is Exist in the form of pentavalent state to obtain vanadium trioxide aqueous slurry, wherein the reaction temperature is 50-300°C, and the hydrogen partial pressure is greater than 1MPa;
三氧化二钒水浆经固液分离后得到三氧化二钒滤饼与滤液；Vanadium trioxide water slurry is separated from solid and liquid to obtain vanadium trioxide filter cake and filtrate;
三氧化二钒滤饼经真空干燥，得到三氧化二钒。The vanadium trioxide filter cake is vacuum-dried to obtain vanadium trioxide.
按上述方案，所述的钒浓度为35～50g/L、含钒溶液中氢离子浓度为10-4～10-7mol/L。According to the above scheme, the vanadium concentration is 35-50 g/L, and the hydrogen ion concentration in the vanadium-containing solution is 10 -4 -10 -7 mol/L.
按上述方案，所述的反应条件为：温度为170～250℃，氢气分压为2.5MPa以上。According to the above scheme, the reaction conditions are as follows: the temperature is 170-250° C., and the hydrogen partial pressure is above 2.5 MPa.
按上述方案，所述的搅拌反应转速为500～1000r/min。According to the above scheme, the stirring reaction speed is 500-1000r/min.
由于采用上述方法，本发明具有以下积极效果：Owing to adopting above-mentioned method, the present invention has following positive effect:
1、由于本发明可直接从含钒溶液中制备出三氧化二钒，与现有工艺相比，省去了由含钒溶液经铵盐沉淀制备中间产品钒酸铵或多聚钒酸铵等的工序，简化了工艺，避免了氨氮废水与氨气的产生；同时，氢气是一种清洁气体，不会造成环境污染，因此本发明具有工艺简单、环境友好的优点；1. Since the present invention can directly prepare vanadium trioxide from the vanadium-containing solution, compared with the prior art, it saves the preparation of intermediate product ammonium vanadate or ammonium polyvanadate etc. by the vanadium-containing solution through ammonium salt precipitation The process simplifies the process and avoids the generation of ammonia-nitrogen wastewater and ammonia; at the same time, hydrogen is a clean gas that will not cause environmental pollution, so the present invention has the advantages of simple process and environmental friendliness;
2、由于本发明所涉及反应为气液反应，温度仅需50～300℃，优选温度在170～250℃，而现有的以偏钒酸铵、多聚钒酸按、五氧化二钒等高价钒产品制备三氧化二钒的工艺所涉及的反应为气固反应，所需温度较高，一般大于500℃，因此，本发明的能耗成本更低；同时，由于本发明简化了工艺，省去了制备偏钒酸铵、多聚钒酸按、五氧化二钒等的工序，进一步降低了生产成本。因此，本发明具有生产成本低的优点。2. Since the reaction involved in the present invention is a gas-liquid reaction, the temperature only needs to be 50-300°C, and the preferred temperature is 170-250°C. The reaction involved in the process of preparing vanadium trioxide from high-priced vanadium products is a gas-solid reaction, and the required temperature is relatively high, generally greater than 500°C. Therefore, the energy consumption cost of the present invention is lower; at the same time, because the present invention simplifies the process, The process of preparing ammonium metavanadate, polyvanadate, vanadium pentoxide and the like is omitted, and the production cost is further reduced. Therefore, the present invention has the advantage of low production costs.
因此，本发明具有工艺简单、环境友好、生产成本低的优点。Therefore, the invention has the advantages of simple process, environmental friendliness and low production cost.
附图说明Description of drawings
图1是本发明的一种工艺流程图。Fig. 1 is a kind of process flow chart of the present invention.
具体实施方式detailed description
下面结合附图和具体实施方式对本发明作进一步的描述，并非对其保护范围的限制：Below in conjunction with accompanying drawing and specific embodiment, the present invention will be further described, not limitation to its protection scope:
本具体实施方式中所述的含钒溶液中的钒以五价态的形式存在。The vanadium in the vanadium-containing solution described in this specific embodiment exists in the form of pentavalent state.
实施例1Example 1
如图1，一种利用含钒溶液制备三氧化二钒的方法。其具体步骤是：As shown in Fig. 1, a method for preparing vanadium trioxide using a vanadium-containing solution. Its specific steps are:
(1)采用氢气与钒浓度为35～50g/L，氢离子浓度为10-4～10-7mol/L的含钒溶液在温度为170～250℃，氢气分压为3～4MPa，搅拌反应转速为800～1000r/min的条件下，于高温高压反应釜中反应3～4小时，得到三氧化二钒水浆；(1) Use a vanadium-containing solution with a hydrogen and vanadium concentration of 35 to 50 g/L and a hydrogen ion concentration of 10 -4 to 10 -7 mol/L at a temperature of 170 to 250°C and a hydrogen partial pressure of 3 to 4 MPa, stirring Under the condition of the reaction speed of 800-1000r/min, react in a high-temperature and high-pressure reactor for 3-4 hours to obtain a vanadium trioxide slurry;
(2)三氧化二钒水浆经固液分离后得到三氧化二钒滤饼与滤液；(2) vanadium trioxide water slurry is obtained vanadium trioxide filter cake and filtrate after solid-liquid separation;
(3)三氧化二钒滤饼经真空干燥，得到三氧化二钒。(3) The vanadium trioxide filter cake is vacuum-dried to obtain vanadium trioxide.
本实施例中三氧化二钒的沉淀率大于98％，三氧化二钒的纯度大于99％。In this embodiment, the precipitation rate of vanadium trioxide is greater than 98%, and the purity of vanadium trioxide is greater than 99%.
实施例2Example 2
一种利用含钒溶液制备三氧化二钒的方法。其具体步骤是：The invention discloses a method for preparing vanadium trioxide from a solution containing vanadium. Its specific steps are:
(1)采用氢气与钒浓度为20～30g/L，氢离子浓度为10-8～10-14mol/L的含钒溶液在温度为100～150℃，氢气分压为2.5～3MPa，搅拌反应转速为500～800r/min的条件下，于高温高压反应釜中反应1～4小时，得到三氧化二钒水浆；(1) Use a vanadium-containing solution with a hydrogen and vanadium concentration of 20 to 30 g/L and a hydrogen ion concentration of 10 -8 to 10 -14 mol/L at a temperature of 100 to 150°C and a hydrogen partial pressure of 2.5 to 3 MPa, stirring Under the condition of the reaction speed of 500-800r/min, react in a high-temperature and high-pressure reactor for 1-4 hours to obtain a vanadium trioxide slurry;
(2)三氧化二钒水浆经固液分离后得到三氧化二钒滤饼与滤液；(2) vanadium trioxide water slurry is obtained vanadium trioxide filter cake and filtrate after solid-liquid separation;
(3)三氧化二钒滤饼经真空干燥，得到三氧化二钒。(3) The vanadium trioxide filter cake is vacuum-dried to obtain vanadium trioxide.
本实施例中三氧化二钒的沉淀率大于98％，三氧化二钒的纯度大于99％。In this embodiment, the precipitation rate of vanadium trioxide is greater than 98%, and the purity of vanadium trioxide is greater than 99%.
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