CN114318014A - A kind of method for double-flow feeding of vanadium slag pressure leaching reaction kettle - Google Patents

A kind of method for double-flow feeding of vanadium slag pressure leaching reaction kettle Download PDF

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CN114318014A
CN114318014A CN202111624946.1A CN202111624946A CN114318014A CN 114318014 A CN114318014 A CN 114318014A CN 202111624946 A CN202111624946 A CN 202111624946A CN 114318014 A CN114318014 A CN 114318014A
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alkali liquor
vanadium
vanadium slag
slurry
reaction kettle
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CN114318014B (en
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刘彪
杜浩
王少娜
吕页清
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Institute of Process Engineering of CAS
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Abstract

The invention provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps: mixing the first alkali liquor and the vanadium slag to obtain slurry; conveying the slurry obtained in the step (1) and the preheated second alkali liquor to a pressurized reaction kettle for oxidation leaching reaction to realize extraction of vanadium; the method adopts a double-flow feeding method to feed materials into the pressurized reaction kettle, thereby not only reducing the loss of conveying equipment, but also improving the leaching rate of vanadium, and leading the leaching rate to reach more than 90 percent and to reach more than 97 percent at most; in addition, the second alkali liquor is preheated by adopting a pipeline preheating mode, so that the energy consumption in the heating process can be saved, and the service life of equipment is prolonged. The method disclosed by the invention is efficient and environment-friendly, is suitable for industrial production, and has a good application prospect.

Description

一种钒渣加压浸出反应釜双流进料的方法A kind of method for double-flow feeding of vanadium slag pressure leaching reaction kettle

技术领域technical field

本发明属于钒化工冶金技术领域,具体涉及一种钒渣加压浸出反应釜双流进料的方法。The invention belongs to the technical field of vanadium chemical industry and metallurgy, and in particular relates to a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle.

背景技术Background technique

钒渣是由含钒铁水在含氧气体存在下吹炼出的一种钒富集物料,钢铁工业中由钒钛磁铁矿生产的钒渣是提钒的主要原料。以钒钛磁铁矿为原料生产铁、钒产品的企业目前都采用传统的钒渣钠化焙烧工艺从钒渣中提钒,如我国的攀钢、承钢,南非海威尔德、新西兰钢铁公司等。钠化焙烧工艺的基本原理是以Na2CO3为添加剂,通过高温钠化焙烧(750-850℃)将低价态的钒转化为水溶性五价钒的钠盐,再对钠化焙烧产物直接水浸,得到含钒的浸取液,后加入铵盐制得多钒酸铵沉淀,经还原焙烧后获得钒的氧化物产品。然而,钠化焙烧工艺钒回收率低,单次焙烧钒回收率为70%左右,经多次焙烧后钒的回收率也仅为80%;且焙烧温度高(750-850℃),并需多次焙烧,能耗偏高;在焙烧过程中还会产生有害的HCl和Cl2等侵蚀性气体,污染环境。因此,提供一种能耗低,工艺流程简单,安全环保的钒渣提钒工艺具有重要的意义。Vanadium slag is a kind of vanadium enriched material smelted from vanadium-containing molten iron in the presence of oxygen-containing gas. Vanadium slag produced from vanadium titanomagnetite in the iron and steel industry is the main raw material for vanadium extraction. Enterprises that use vanadium titanomagnetite as raw materials to produce iron and vanadium products currently use the traditional vanadium slag sodium roasting process to extract vanadium from vanadium slag, such as my country's Pangang and Chenggang, South Africa's Highveld, New Zealand's Steel company etc. The basic principle of the sodium roasting process is to use Na 2 CO 3 as an additive, and through high temperature sodium roasting (750-850 ℃), the low-valence vanadium is converted into the sodium salt of water-soluble pentavalent vanadium, and then the sodium roasting product is Direct water leaching to obtain vanadium-containing leaching solution, then adding ammonium salt to prepare ammonium polyvanadate precipitation, and obtaining vanadium oxide product after reduction roasting. However, the recovery rate of vanadium in the sodium roasting process is low, the recovery rate of vanadium in a single roasting is about 70%, and the recovery rate of vanadium after multiple roasting is only 80%; and the roasting temperature is high (750-850 ° C), and requires Repeated roasting will result in high energy consumption; in the roasting process, harmful corrosive gases such as HCl and Cl 2 will also be produced, polluting the environment. Therefore, it is of great significance to provide a vanadium extraction process from vanadium slag with low energy consumption, simple process flow, safety and environmental protection.

CN102531056A公开了一种钒渣加压浸出加压反应釜的方法,该方法先将NaOH溶液与钒渣在配制罐内进行搅拌混合,配制成液固比4-6:1的浆料,然后通过耐碱、耐高温、耐磨损的泵全部输送至加压加压反应釜中进行浸出反应。但该方法对设备要求比较高,设备的腐蚀磨损比较严重,而且采用单一进料泵的方式进料,进料时间长,加压反应釜内还需要增加升温装置,增加了设备成本的同时,还延长了整个反应周期,能耗较高。CN102531056A discloses a method for pressurized leaching of vanadium slag in a pressurized reactor. The method firstly stirs and mixes NaOH solution and vanadium slag in a preparation tank to prepare a slurry with a liquid-solid ratio of 4-6:1, and then passes All the pumps with alkali resistance, high temperature resistance and wear resistance are transported to the pressurized and pressurized reactor for leaching reaction. However, this method has relatively high requirements on the equipment, and the corrosion and wear of the equipment is relatively serious, and the feeding time is long by using a single feeding pump. The whole reaction cycle is also prolonged, and the energy consumption is higher.

CN110760687A公开了一种低成本钒渣清洁提钒的方法,包括钒渣焙烧、碱浸、净化和沉钒四个步骤,钒渣和氧化钙混合后焙烧得到焙烧熟料,焙烧熟料通过碱浸得到残渣和含钒浸出液,残渣清洗后洗液浓缩与含钒浸出液混合得到含钒混合液,含钒混合液与氯化钙得到钒酸钠溶液,钒酸钠溶液通过加入氯化铵溶液固液分离得到偏钒酸铵沉淀和沉钒废水,沉钒废水返回碱浸步骤用于焙烧熟料的碱性浸取。该方法虽未采用钠化焙烧工艺,而是与氧化钙混合焙烧,但其焙烧温度同样较高,能耗偏高。CN110760687A discloses a low-cost vanadium slag cleaning and vanadium extraction method, which includes four steps of vanadium slag roasting, alkali leaching, purification and vanadium precipitation. The vanadium slag and calcium oxide are mixed and roasted to obtain roasted clinker, and the roasted clinker is subjected to alkali leaching. The residue and vanadium-containing leachate are obtained. After the residue is washed, the washing solution is concentrated and mixed with the vanadium-containing leachate to obtain a vanadium-containing mixed solution. The vanadium-containing mixed solution is mixed with calcium chloride to obtain a sodium vanadate solution. The sodium vanadate solution is added to the solid-liquid ammonium chloride solution The ammonium metavanadate precipitation and the vanadium precipitation wastewater are obtained by separation, and the vanadium precipitation wastewater is returned to the alkaline leaching step for alkaline leaching of the roasting clinker. Although this method does not use the sodium roasting process, but is mixed with calcium oxide for roasting, the roasting temperature is also high, and the energy consumption is relatively high.

综上所述,如何提供一种能耗低,工艺流程简单,安全环保的钒渣提钒工艺成为当前亟待解决的问题。In summary, how to provide a vanadium extraction process from vanadium slag with low energy consumption, simple process flow, safety and environmental protection has become an urgent problem to be solved at present.

发明内容SUMMARY OF THE INVENTION

针对现有技术存在的问题,本发明的目的在于提供一种钒渣加压浸出反应釜双流进料的方法,所述方法采用双流进料的方式,极大地降低了料浆对设备的损耗,所述方法高效环保,适用于工业化生产。In view of the problems existing in the prior art, the object of the present invention is to provide a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle. The method is efficient and environmentally friendly, and is suitable for industrial production.

为达此目的,本发明采用以下技术方案:For this purpose, the present invention adopts the following technical solutions:

本发明提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The invention provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, the method comprises the following steps:

(1)将第一碱液与钒渣混合,得到浆料;(1) the first alkali liquor is mixed with vanadium slag to obtain slurry;

(2)将步骤(1)得到的浆料与预热后的第二碱液输送至加压反应釜中进行氧化浸出反应,实现钒的提取。(2) The slurry obtained in step (1) and the preheated second lye solution are transported to a pressurized reaction kettle for oxidative leaching reaction to realize the extraction of vanadium.

本发明中,第一碱液和第二碱液可为同一碱液分为的两股,也可分别独立地配制。In the present invention, the first lye solution and the second lye solution may be divided into two strands of the same lye solution, or may be prepared independently.

本发明中,优化了传统的先配料后进料的方法,将碱液进行分流,一部分先与钒渣形成浆料,另一部分再与形成的浆料进行双流进料,采用该方法可有效较低料流对输送泵的损耗,延长设备的使用寿命,节能高效,具有较好的经济效益,有利于工业化应用。In the present invention, the traditional method of first batching and then feeding is optimized, the lye is divided into two streams, one part is formed into a slurry with vanadium slag, and the other part is then fed with the formed slurry in two streams. This method can effectively compare The loss of low material flow to the conveying pump can prolong the service life of the equipment, save energy and high efficiency, and has good economic benefits, which is conducive to industrial application.

以下作为本发明优选的技术方案,但不作为本发明提供的技术方案的限制,通过以下技术方案,可以更好地达到和实现本发明的技术目的和有益效果。The following are the preferred technical solutions of the present invention, but not as limitations of the technical solutions provided by the present invention. Through the following technical solutions, the technical purpose and beneficial effects of the present invention can be better achieved and realized.

作为本发明优选的技术方案,步骤(1)所述第一碱液包括NaOH溶液。As a preferred technical solution of the present invention, the first alkali solution in step (1) includes NaOH solution.

优选地,步骤(1)所述第一碱液包括新鲜碱液和/或经过蒸发浓缩后的循环碱液。Preferably, the first alkali liquor in step (1) includes fresh alkali liquor and/or circulating alkali liquor after evaporation and concentration.

优选地,步骤(1)所述的第一碱液的浓度为40-50wt%,例如40wt%、41wt%、42wt%、43wt%、44wt%、45wt%、46wt%、47wt%、48wt%、49wt%或50wt%等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the concentration of the first alkali solution in step (1) is 40-50wt%, such as 40wt%, 41wt%, 42wt%, 43wt%, 44wt%, 45wt%, 46wt%, 47wt%, 48wt%, 49 wt % or 50 wt %, etc., but not limited to the recited values, and other unrecited values within the numerical range are also applicable.

优选地,步骤(1)所述的第一碱液的初始温度为80-120℃,例如80℃、85℃、90℃、95℃、100℃、105℃、110℃、115℃或120℃等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the initial temperature of the first alkali solution in step (1) is 80-120°C, such as 80°C, 85°C, 90°C, 95°C, 100°C, 105°C, 110°C, 115°C or 120°C etc., but are not limited to the recited numerical values, and other unrecited numerical values within the numerical range are equally applicable.

作为本发明优选的技术方案,步骤(1)所述钒渣中过200目筛的颗粒占比为70-90wt%,例如70wt%、72wt%、74wt%、76wt%、78wt%、80wt%、82wt%、84wt%、86wt%、88wt%或90wt%等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。As a preferred technical solution of the present invention, the proportion of particles passing through a 200-mesh sieve in the vanadium slag in step (1) is 70-90wt%, such as 70wt%, 72wt%, 74wt%, 76wt%, 78wt%, 80wt%, 82 wt %, 84 wt %, 86 wt %, 88 wt % or 90 wt %, etc., but not limited to the recited values, and other unrecited values within the numerical range are also applicable.

作为本发明优选的技术方案,步骤(1)所述浆料的液固比为(1.0-2):1,例如1.0:1、1.1:1、1.2:1、1.3:1、1.4:1、1.5:1、1.6:1、1.7:1、1.8:1、1.9:1或2:1等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。As a preferred technical solution of the present invention, the liquid-solid ratio of the slurry in step (1) is (1.0-2):1, such as 1.0:1, 1.1:1, 1.2:1, 1.3:1, 1.4:1, 1.5:1, 1.6:1, 1.7:1, 1.8:1, 1.9:1 or 2:1, etc., but not limited to the listed values, and other unlisted values within the numerical range are also applicable.

优选地,步骤(1)所述浆料的温度不超过95℃,例如80℃、82℃、84℃、86℃、88℃、90℃、93℃或95℃等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the temperature of the slurry in step (1) does not exceed 95°C, such as 80°C, 82°C, 84°C, 86°C, 88°C, 90°C, 93°C, or 95°C, etc., but not limited to those listed value, other non-recited values within this value range also apply.

本发明中,步骤(2)的浆料采用隔膜泵进行输送,是由于隔膜泵无轴封、无泄漏、流道宽敞、没有叶轮、泵自身部件磨损小,所以输送含颗粒,易挥发和腐蚀性介质时,不会造成环境污染和危害人身安全。但隔膜泵对进料温度有要求,不得高于95℃,因此浆料的液固比十分重要,本发明所述方法通过调整液固比,从而控制浆料温度。若液固比过大,会导致浆料温度过高,超过95℃将加剧隔膜泵腐蚀,影响使用寿命;若液固比过小,则浆料固含量太高,浆料无法正常输送,容易堵塞进料管道。In the present invention, the slurry in step (2) is transported by a diaphragm pump, because the diaphragm pump has no shaft seal, no leakage, wide flow channel, no impeller, and small wear of the pump itself, so the transport contains particles, which are easy to volatilize and corrode When using a sexual medium, it will not cause environmental pollution and endanger personal safety. However, the diaphragm pump has requirements on the feeding temperature, which should not be higher than 95°C, so the liquid-solid ratio of the slurry is very important. The method of the present invention controls the slurry temperature by adjusting the liquid-solid ratio. If the liquid-solid ratio is too large, the slurry temperature will be too high. If the temperature exceeds 95°C, the diaphragm pump will be corroded and the service life will be affected. If the liquid-solid ratio is too small, the solid content of the slurry will be too high, and the slurry cannot be transported normally. Blocked feed line.

作为本发明优选的技术方案,步骤(2)所述第二碱液包括NaOH溶液。As a preferred technical solution of the present invention, the second alkali solution in step (2) includes NaOH solution.

优选地,步骤(2)所述第二碱液包括新鲜碱液和/或经过蒸发浓缩后的循环碱液。Preferably, the second alkali liquor in step (2) includes fresh alkali liquor and/or circulating alkali liquor after evaporation and concentration.

优选地,步骤(2)所述的第二碱液的浓度为40-50wt%,例如40wt%、41wt%、42wt%、43wt%、44wt%、45wt%、46wt%、47wt%、48wt%、49wt%或50wt%等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the concentration of the second alkali solution in step (2) is 40-50wt%, such as 40wt%, 41wt%, 42wt%, 43wt%, 44wt%, 45wt%, 46wt%, 47wt%, 48wt%, 49 wt % or 50 wt %, etc., but not limited to the recited values, and other unrecited values within the numerical range are also applicable.

优选地,步骤(2)所述的第二碱液的初始温度为80-120℃,例如80℃、85℃、90℃、95℃、100℃、105℃、110℃、115℃或120℃等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the initial temperature of the second alkali solution in step (2) is 80-120°C, such as 80°C, 85°C, 90°C, 95°C, 100°C, 105°C, 110°C, 115°C or 120°C etc., but are not limited to the recited numerical values, and other unrecited numerical values within the numerical range are equally applicable.

作为本发明优选的技术方案,步骤(2)所述第二碱液采用管道预热器进行预热。As a preferred technical solution of the present invention, the second alkali solution in step (2) is preheated by a pipeline preheater.

优选地,所述管道预热器采用的加热介质包括饱和蒸汽。Preferably, the heating medium used by the pipeline preheater includes saturated steam.

优选地,所述饱和蒸汽的压力不小于2.0MPa,例如2.0MPa、2.2MPa、2.3MPa、2.5MPa、3.0MPa、3.2MPa、3.5MPa、3.8MPa或4.0MPa等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the pressure of the saturated steam is not less than 2.0 MPa, such as 2.0 MPa, 2.2 MPa, 2.3 MPa, 2.5 MPa, 3.0 MPa, 3.2 MPa, 3.5 MPa, 3.8 MPa or 4.0 MPa, etc., but not limited to those listed Numerical values, other non-recited values within the numerical range also apply.

优选地,步骤(2)所述第二碱液预热后的温度为180-220℃,例如180℃、185℃、190℃、195℃、200℃、205℃、210℃、215℃或220℃等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the preheated temperature of the second lye solution in step (2) is 180-220°C, such as 180°C, 185°C, 190°C, 195°C, 200°C, 205°C, 210°C, 215°C or 220°C °C, etc., but are not limited to the listed numerical values, and other unlisted numerical values within the numerical range are also applicable.

本发明中,传统加压氧化反应采用蒸汽直接加热或者电磁感应加热,蒸汽直接加热会导致反应釜碱液浆料被稀释,进而影响钒的提取效果;电磁感应加热则通过加热反应釜釜体,釜体再将热量传递给浆料,釜体散热大、热效率低,而且电加热的能耗成本较蒸汽更高。而本发明蒸汽管道化预热不仅可以提高蒸汽加热换热效率、降低预热成本,而且通过蒸汽间接换热不会影响浆液碱浓度,是一种高效、节能的加热方法。In the present invention, the traditional pressurized oxidation reaction adopts steam direct heating or electromagnetic induction heating. Direct steam heating will cause the lye slurry of the reactor to be diluted, thereby affecting the extraction effect of vanadium; The kettle body then transfers the heat to the slurry. The kettle body has large heat dissipation and low thermal efficiency, and the energy consumption cost of electric heating is higher than that of steam. The steam pipeline preheating of the invention can not only improve the heat exchange efficiency of steam heating and reduce the preheating cost, but also does not affect the alkali concentration of the slurry through the indirect heat exchange of the steam, and is an efficient and energy-saving heating method.

作为本发明优选的技术方案,步骤(2)所述第二碱液的加入量是步骤(1)所述钒渣质量的3-5倍,例如3.0倍、3.2倍、3.4倍、3.6倍、3.8倍、4.0倍、4.2倍、4.4倍、4.6倍、4.8倍或5.0倍等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。As a preferred technical solution of the present invention, the added amount of the second alkali solution described in step (2) is 3-5 times the mass of the vanadium slag described in step (1), such as 3.0 times, 3.2 times, 3.4 times, 3.6 times, 3.8 times, 4.0 times, 4.2 times, 4.4 times, 4.6 times, 4.8 times, or 5.0 times, etc., but not limited to the listed numerical values, and other unlisted numerical values within the numerical range are also applicable.

作为本发明优选的技术方案,步骤(2)所述浆料采用隔膜泵进行输送。As a preferred technical solution of the present invention, the slurry in step (2) is transported by a diaphragm pump.

优选地,步骤(2)所述第二碱液采用离心泵进行输送。Preferably, the second alkali solution in step (2) is transported by a centrifugal pump.

优选地,所述离心泵的叶轮材质包括Ni基合金。Preferably, the impeller material of the centrifugal pump includes Ni-based alloy.

优选地,所述Ni基合金包括Ni-Cr合金、Ni-Cr-Mo-Cu合金、Ni-Cr-Mo(W)合金或Ni-Cr-W合金中的任意一种,优选为Ni-Cr合金。Preferably, the Ni-based alloy includes any one of Ni-Cr alloy, Ni-Cr-Mo-Cu alloy, Ni-Cr-Mo(W) alloy or Ni-Cr-W alloy, preferably Ni-Cr alloy.

作为本发明优选的技术方案,步骤(2)所述氧化浸出反应的压力为0.6-1.0MPa,例如0.60MPa、0.65MPa、0.70MPa、0.75MPa、0.80MPa、0.85MPa、0.90MPa、0.95MPa或1.00MPa等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。As a preferred technical solution of the present invention, the pressure of the oxidative leaching reaction in step (2) is 0.6-1.0 MPa, such as 0.60 MPa, 0.65 MPa, 0.70 MPa, 0.75 MPa, 0.80 MPa, 0.85 MPa, 0.90 MPa, 0.95 MPa or 1.00 MPa, etc., but not limited to the listed numerical values, and other unlisted numerical values within the numerical range are also applicable.

优选地,步骤(2)所述氧化浸出反应的温度为160-180℃,例如160℃、163℃、166℃、169℃、172℃、175℃、178℃或180℃等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the temperature of the oxidative leaching reaction in step (2) is 160-180°C, such as 160°C, 163°C, 166°C, 169°C, 172°C, 175°C, 178°C or 180°C, etc., but not limited to Recited values apply equally well to other non-recited values within this range of values.

本发明中,预热后的第二碱液与浆料混合后温度即可达到设定反应温度160-180℃,反应釜无需增加加热装备,通过氧化浸出过程的反应放热即可保证浸出温度,从而节约能耗,降低反应釜设备投资。In the present invention, the temperature of the preheated second lye solution and the slurry can reach the set reaction temperature of 160-180° C. The reaction kettle does not need to add heating equipment, and the leaching temperature can be guaranteed by the reaction exotherm of the oxidative leaching process. , thereby saving energy consumption and reducing investment in reactor equipment.

优选地,步骤(2)所述氧化浸出反应采用的氧化性气体包括氧气、空气或臭氧中的任意一种或至少两种的组合。Preferably, the oxidizing gas used in the oxidative leaching reaction in step (2) includes any one or a combination of at least two of oxygen, air or ozone.

优选地,步骤(2)所述氧化浸出反应的氧分压为0.3-0.5MPa,例如0.30MPa、0.33MPa、0.36MPa、0.39MPa、0.42MPa、0.45MPa、0.48MPa、或0.50MPa等,但并不仅限于所列举的数值,该数值范围内其他未列举的数值同样适用。Preferably, the oxygen partial pressure of the oxidative leaching reaction in step (2) is 0.3-0.5 MPa, such as 0.30 MPa, 0.33 MPa, 0.36 MPa, 0.39 MPa, 0.42 MPa, 0.45 MPa, 0.48 MPa, or 0.50 MPa, etc., but Not limited to the recited values, other non-recited values within the range of values apply equally.

作为本发明优选的技术方案,所述方法包括以下步骤:As the preferred technical solution of the present invention, the method comprises the following steps:

(1)将初始温度为80-120℃、浓度为40-50wt%第一碱液与过200目筛颗粒占比为70-90wt%的钒渣混合,得到液固比为(1-2):1的浆料;(1) Mix the first alkali solution with an initial temperature of 80-120°C and a concentration of 40-50wt% and vanadium slag with a particle ratio of 70-90wt% passing through a 200-mesh sieve to obtain a liquid-solid ratio of (1-2) :1 slurry;

(2)采用管道预热器将第二碱液预热至180-220℃,其中,加热介质为压力不小于2.0MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second alkali liquid to 180-220°C, wherein the heating medium is saturated steam with a pressure of not less than 2.0MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二碱液利用离心泵输送至加压反应釜中,所述第二碱液的加入量为步骤(1)所述钒渣质量的3-5倍,二者混合后在0.6-1.0MPa、160-180℃、氧分压为0.3-0.5MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported to the reactor by a diaphragm pump, and the preheated second lye is transported to the pressurized reactor by a centrifugal pump. The addition amount of the second lye It is 3-5 times the quality of the vanadium slag described in step (1), and after mixing the two, the oxidation leaching reaction is carried out under the conditions of 0.6-1.0MPa, 160-180 ° C, and oxygen partial pressure of 0.3-0.5MPa, so as to realize the vanadium leaching reaction. extract.

与现有技术相比,本发明具有以下有益效果:Compared with the prior art, the present invention has the following beneficial effects:

(1)本发明所述的钒渣加压浸出反应釜双流进料方法,优化了传统的先配料后进料的方法,将部分碱液与钒渣混合形成浆料,再将另一部分碱液与得到的浆料实现双流进料,使进料过程更简单高效;(1) the vanadium slag pressurized leaching reaction kettle double-flow feeding method of the present invention optimizes the traditional method of first batching and then feeding, mixing part of the lye with the vanadium slag to form a slurry, and then mixing another part of the lye Realize dual-stream feeding with the obtained slurry, making the feeding process simpler and more efficient;

(2)本发明所述方法通过配制低液固比的钒渣浆料控制浆料温度不超过95℃,从而满足隔膜泵对物料输送温度的要求,保证钒渣浆料可以采用经久耐用的隔膜泵作为加压反应釜进料泵;(2) The method of the present invention controls the temperature of the slurry to not exceed 95°C by preparing a vanadium slag slurry with a low liquid-solid ratio, so as to meet the requirements of the diaphragm pump for the material conveying temperature, and ensure that the vanadium slag slurry can use a durable diaphragm The pump is used as the feed pump for the pressurized reactor;

(3)本发明所述方法利用隔膜泵对浆料输送到反应釜中,能够避免浆料对传统输送泵叶轮的损耗,延长设备的使用周期;(3) The method of the present invention utilizes the diaphragm pump to transport the slurry to the reaction kettle, which can avoid the loss of the slurry to the impeller of the traditional transport pump and prolong the service life of the equipment;

(4)本发明所述方法采用管道化预热的方式将第二碱液预热到反应温度,由于液碱中不含有固体颗粒,输送碱液的泵叶轮磨损大幅降低,同样可使其使用寿命可明显延长;(4) The method of the present invention adopts the pipeline preheating method to preheat the second lye to the reaction temperature. Since the liquid caustic does not contain solid particles, the wear of the impeller of the pump for transporting the lye is greatly reduced, and it can also be used. The lifespan can be significantly extended;

(5)本发明所述方法的第二碱液采用蒸汽管道化预热的方法加热,不仅可以提高蒸汽加热换热效率、降低预热成本,而且蒸汽间接换热不会影响浆液碱浓度,是一种高效、节能的加热方法;(5) The second alkali liquid of the method of the present invention is heated by the method of steam pipeline preheating, which can not only improve the heat exchange efficiency of steam heating and reduce the preheating cost, but also the indirect heat exchange of steam will not affect the alkali concentration of the slurry. An efficient and energy-saving heating method;

(6)本发明所述方法可使钒的回收率达90%以上,最高可达97%以上。(6) The method of the present invention can make the recovery rate of vanadium reach more than 90%, and the highest can reach more than 97%.

附图说明Description of drawings

图1是本发明实施例1提供的一种钒渣加压浸出反应釜双流进料方法工艺流程图。Fig. 1 is the process flow diagram of a kind of vanadium slag pressure leaching reaction kettle double-stream feeding method provided in the embodiment 1 of the present invention.

具体实施方式Detailed ways

为更好地说明本发明,便于理解本发明的技术方案,下面对本发明进一步详细说明。但下述的实施例仅是本发明的简易例子,并不代表或限制本发明的权利保护范围,本发明保护范围以权利要求书为准。In order to better illustrate the present invention and facilitate understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following embodiments are only simple examples of the present invention, and do not represent or limit the protection scope of the present invention, and the protection scope of the present invention is subject to the claims.

以下为本发明典型但非限制性实施例:The following are typical but non-limiting examples of the present invention:

实施例1:Example 1:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法的工艺流程如图1所示。The present embodiment provides a method for double-flow feeding of vanadium slag pressurized leaching reaction kettle, and the process flow of the method is shown in FIG. 1 .

所述方法包括以下步骤:The method includes the following steps:

提供初始温度为90℃、浓度为45wt%的蒸发后的循环NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide an evaporated circulating NaOH solution with an initial temperature of 90 °C and a concentration of 45 wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为80wt%的钒渣混合,得到液固比为1.6:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 80 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.6:1;

(2)采用管道预热器将第二NaOH溶液预热至180℃,其中,加热介质为压力为3.0MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 180°C, wherein the heating medium is saturated steam with a pressure of 3.0MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的3.4倍,二者混合后在0.8MPa、160℃、氧分压为0.4MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported into the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported into the pressurized reaction kettle by a centrifugal pump whose impeller material is Ni-Cr alloy, so that the The added amount of the second NaOH solution is 3.4 times the quality of the vanadium slag described in step (1). After the two are mixed, the oxidative leaching reaction is carried out under the conditions of 0.8MPa, 160° C., and an oxygen partial pressure of 0.4MPa to achieve vanadium extract.

实施例2:Example 2:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为86℃、浓度为48wt%的新鲜配制的NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide a freshly prepared NaOH solution with an initial temperature of 86 ° C and a concentration of 48 wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为84wt%的钒渣混合,得到液固比为2.0:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 84 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 2.0:1;

(2)采用管道预热器将第二NaOH溶液预热至210℃,其中,加热介质为压力3.6MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 210°C, wherein the heating medium is saturated steam with a pressure of 3.6MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的3.0倍,二者混合后在0.8MPa、175℃、氧分压为0.45MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported into the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported into the pressurized reaction kettle by a centrifugal pump whose impeller material is Ni-Cr alloy, so that the The added amount of the second NaOH solution is 3.0 times the mass of the vanadium slag described in step (1). extract.

实施例3:Example 3:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为80℃、浓度为50wt%的蒸发后的循环NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide an evaporated circulating NaOH solution with an initial temperature of 80°C and a concentration of 50wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为86wt%的钒渣混合,得到液固比为1.8:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 86 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.8:1;

(2)采用管道预热器将第二NaOH溶液预热至220℃,其中,加热介质为压力3.7MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 220°C, wherein the heating medium is saturated steam with a pressure of 3.7MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr-Mo-Cu合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的3.2倍,二者混合后在0.8MPa、180℃、氧分压为0.50MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported to the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported to the pressurized reaction by a centrifugal pump whose impeller material is Ni-Cr-Mo-Cu alloy In the kettle, the added amount of the second NaOH solution is 3.2 times the quality of the vanadium slag described in step (1), and after mixing the two, the oxidative leaching reaction is carried out under the conditions of 0.8 MPa, 180 ° C, and an oxygen partial pressure of 0.50 MPa , to achieve vanadium extraction.

实施例4:Example 4:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为88℃、浓度为48wt%的新鲜配制的NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide a freshly prepared NaOH solution with an initial temperature of 88 °C and a concentration of 48 wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为76wt%的钒渣混合,得到液固比为1.0:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 76 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.0:1;

(2)采用管道预热器将第二NaOH溶液预热至215℃,其中,加热介质为压力3.0MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 215°C, wherein the heating medium is saturated steam with a pressure of 3.0MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的4.0倍,二者混合后在0.9MPa、178℃、氧分压为0.40MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported into the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported into the pressurized reaction kettle by a centrifugal pump whose impeller material is Ni-Cr alloy, so that the The added amount of the second NaOH solution is 4.0 times the mass of the vanadium slag described in step (1). extract.

实施例5:Example 5:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为110℃、浓度为47wt%的蒸发后的循环NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide an evaporated circulating NaOH solution with an initial temperature of 110° C. and a concentration of 47wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为70wt%的钒渣混合,得到液固比为1.4:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 70 wt % passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.4:1;

(2)采用管道预热器将第二NaOH溶液预热至200℃,其中,加热介质为压力2.0MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 200°C, wherein the heating medium is saturated steam with a pressure of 2.0MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的3.6倍,二者混合后在0.92MPa、170℃、氧分压为0.38MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported into the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported into the pressurized reaction kettle by a centrifugal pump whose impeller material is Ni-Cr alloy, so that the The added amount of the second NaOH solution is 3.6 times the mass of the vanadium slag described in step (1). extract.

实施例6:Example 6:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为105℃、浓度为48wt%的蒸发后的循环NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide an evaporated circulating NaOH solution with an initial temperature of 105° C. and a concentration of 48wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为88wt%的钒渣混合,得到液固比为1.5:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 88 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.5:1;

(2)采用管道预热器将第二NaOH溶液预热至190℃,其中,加热介质为压力3.2MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 190°C, wherein the heating medium is saturated steam with a pressure of 3.2MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的3.5倍,二者混合后在0.95MPa、165℃、氧分压为0.35MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported into the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported into the pressurized reaction kettle by a centrifugal pump whose impeller material is Ni-Cr alloy, so that the The added amount of the second NaOH solution is 3.5 times the mass of the vanadium slag described in step (1). After the two are mixed, the oxidative leaching reaction is carried out under the conditions of 0.95MPa, 165° C., and an oxygen partial pressure of 0.35MPa to achieve vanadium extract.

实施例7:Example 7:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为90℃、浓度为46wt%的蒸发后的循环NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide an evaporated circulating NaOH solution with an initial temperature of 90° C. and a concentration of 46 wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为72wt%的钒渣混合,得到液固比为1.3:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 72 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.3:1;

(2)采用管道预热器将第二NaOH溶液预热至185℃,其中,加热介质为压力2.5MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 185°C, wherein the heating medium is saturated steam with a pressure of 2.5MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr-Mo合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的3.7倍,二者混合后在0.75MPa、163℃、氧分压为0.30MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported to the reactor by a diaphragm pump, and the preheated second NaOH solution is transported to the pressurized reactor by a centrifugal pump whose impeller material is Ni-Cr-Mo alloy , the added amount of the second NaOH solution is 3.7 times the mass of the vanadium slag described in step (1), and after the two are mixed, the oxidative leaching reaction is carried out under the conditions of 0.75MPa, 163 ° C, and an oxygen partial pressure of 0.30MPa to achieve Extraction of vanadium.

实施例8:Example 8:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为120℃、浓度为50wt%的蒸发后的循环NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide an evaporated circulating NaOH solution with an initial temperature of 120 ° C and a concentration of 50 wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为90wt%的钒渣混合,得到液固比为1.0:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 90 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.0:1;

(2)采用管道预热器将第二NaOH溶液预热至220℃,其中,加热介质为压力4.0MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 220°C, wherein the heating medium is saturated steam with a pressure of 4.0MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的4.0倍,二者混合后在1.0MPa、180℃、氧分压为0.5MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported into the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported into the pressurized reaction kettle by a centrifugal pump whose impeller material is Ni-Cr alloy, so that the The added amount of the second NaOH solution is 4.0 times the quality of the vanadium slag described in step (1). extract.

实施例9:Example 9:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法包括以下步骤:The present embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle, and the method comprises the following steps:

提供初始温度为80℃、浓度为45wt%的蒸发后的循环NaOH溶液,将其分为A股和B股,其中,A股为第一NaOH溶液,B股为第二NaOH溶液;Provide an evaporated circulating NaOH solution with an initial temperature of 80 °C and a concentration of 45 wt%, and divide it into A shares and B shares, wherein the A shares are the first NaOH solution, and the B shares are the second NaOH solution;

(1)将第一NaOH溶液与过200目筛颗粒占比为74wt%的钒渣混合,得到液固比为1.9:1的浆料;(1) mixing the first NaOH solution with the vanadium slag with a particle ratio of 74 wt% passing through a 200-mesh sieve to obtain a slurry with a liquid-solid ratio of 1.9:1;

(2)采用管道预热器将第二NaOH溶液预热至180℃,其中,加热介质为压力3.5MPa的饱和蒸汽;(2) using a pipeline preheater to preheat the second NaOH solution to 180°C, wherein the heating medium is saturated steam with a pressure of 3.5MPa;

然后,将步骤(1)得到的浆料采用隔膜泵输送至反应釜中,并将预热后的第二NaOH溶液利用叶轮材质为Ni-Cr合金的离心泵输送至加压反应釜中,所述第二NaOH溶液的加入量为步骤(1)所述钒渣质量的3.1倍,二者混合后在0.60MPa、160℃、氧分压为0.30MPa的条件下进行氧化浸出反应,实现钒的提取。Then, the slurry obtained in step (1) is transported into the reaction kettle by a diaphragm pump, and the preheated second NaOH solution is transported into the pressurized reaction kettle by a centrifugal pump whose impeller material is Ni-Cr alloy, so that the The added amount of the second NaOH solution is 3.1 times the mass of the vanadium slag described in step (1). After the two are mixed, the oxidation leaching reaction is carried out under the conditions of 0.60 MPa, 160 ° C, and an oxygen partial pressure of 0.30 MPa, so as to realize the vanadium extract.

实施例10:Example 10:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法参照实施例4中方法,区别仅在于:步骤(1)中得到的浆料的液固比为0.5:1。The present embodiment provides a method for dual-stream feeding of vanadium slag pressurized leaching reactor, and the method refers to the method in Example 4, and the difference is only that: the liquid-solid ratio of the slurry obtained in step (1) is 0.5: 1.

实施例11:Example 11:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法参照实施例2中方法,区别仅在于:步骤(1)中得到的浆料的液固比为2.5:1。The present embodiment provides a method for dual-stream feeding of vanadium slag pressurized leaching reactor, and the method refers to the method in Example 2, and the difference is only that: the liquid-solid ratio of the slurry obtained in step (1) is 2.5: 1.

实施例12:Example 12:

本实施例提供了一种钒渣加压浸出反应釜双流进料的方法,所述方法参照实施例1中方法,区别仅在于:步骤(2)中离心泵的叶轮材质为316L不锈钢。This embodiment provides a method for double-flow feeding of vanadium slag pressure leaching reaction kettle. The method refers to the method in Example 1, except that the impeller of the centrifugal pump in step (2) is made of 316L stainless steel.

测定实施例1-12中钒的浸出率,结果如表1所示。The leaching rate of vanadium in Examples 1-12 was measured, and the results are shown in Table 1.

表1Table 1

Figure BDA0003439644430000131
Figure BDA0003439644430000131

Figure BDA0003439644430000141
Figure BDA0003439644430000141

实施例1-9采用本发明所述方法,通过优化进料方式,提高设备使用寿命的同时保证了钒的浸出率,使其达90%以上,最高可达97%以上;实施例10中第一碱液与钒渣混合形成的浆料液固比过小,导致浆料输送非常困难,进料管道堵塞频率非常高;实施例11中第一碱液与钒渣混合形成的浆料液固比过大,导致浆料温度达到110℃,隔膜泵中橡胶隔膜的使用寿命由一年缩短为3个月;实施例12中输送第二碱液的离心泵叶轮材质为常规的316L不锈钢材质,虽然对钒的浸出率没有影响,但离心泵叶轮的使用寿命由6个月缩短到2个月,提高了设备成本。Embodiments 1-9 adopt the method of the present invention, and by optimizing the feeding method, the service life of the equipment is improved, and the leaching rate of vanadium is ensured to reach more than 90%, and the maximum can reach more than 97%; The liquid-solid ratio of the slurry formed by mixing alkali liquor and vanadium slag is too small, which makes the slurry transportation very difficult, and the frequency of blockage of the feed pipeline is very high; in Example 11, the slurry liquid-solid ratio formed by mixing the first alkali liquor and vanadium slag If the ratio is too large, the temperature of the slurry reaches 110 °C, and the service life of the rubber diaphragm in the diaphragm pump is shortened from one year to 3 months; Although it has no effect on the vanadium leaching rate, the service life of the impeller of the centrifugal pump is shortened from 6 months to 2 months, which increases the equipment cost.

综合上述实施例可以看出,第一方面,本发明所述的钒渣加压浸出反应釜双流进料方法,优化了传统的先配料后进料的方法,将部分碱液与钒渣混合形成浆料,再将另一部分碱液与得到的浆料实现双流进料,使进料过程更简单高效;第二方面,所述方法通过配制低液固比的钒渣浆料控制浆料温度不超过95℃,从而满足隔膜泵对物料输送温度的要求,保证钒渣浆料可以采用经久耐用的隔膜泵作为加压反应釜进料泵;第三方面,所述方法利用隔膜泵对浆料输送到反应釜中,能够避免浆料对传统输送泵叶轮的损耗,延长设备的使用周期,所述方法还采用管道化预热的方式将第二碱液预热到反应温度,由于液碱中不含有固体颗粒,输送碱液的泵叶轮磨损大幅降低,同样可使其使用寿命可明显延长;第四方面,所述方法的第二碱液采用蒸汽管道化预热的方法加热,不仅可以提高蒸汽加热换热效率、降低预热成本,而且蒸汽间接换热不会影响浆液碱浓度,是一种高效、节能的加热方法;第五方面,所述方法保证的钒的浸出率,可其可达90%以上,最高可达97%以上。It can be seen from the above examples that, in the first aspect, the double-stream feeding method of the vanadium slag pressurized leaching reaction kettle of the present invention optimizes the traditional method of first batching and then feeding, and mixes part of the lye with the vanadium slag to form Slurry, and then another part of the lye and the obtained slurry are fed into two streams, so that the feeding process is simpler and more efficient; in the second aspect, the method controls the temperature of the slurry by preparing a vanadium slag slurry with a low liquid-solid ratio. The temperature exceeds 95 °C, so as to meet the requirements of the diaphragm pump for the material conveying temperature, and ensure that the vanadium slag slurry can use a durable diaphragm pump as the feed pump for the pressurized reaction kettle; thirdly, the method uses the diaphragm pump to transport the slurry. In the reaction kettle, it can avoid the loss of the impeller of the traditional conveying pump and prolong the service life of the equipment. The method also adopts the pipeline preheating method to preheat the second lye to the reaction temperature. Containing solid particles, the wear of the impeller of the pump transporting the lye is greatly reduced, and the service life of the pump can also be significantly prolonged; in the fourth aspect, the second lye of the method is heated by the method of steam pipeline preheating, which can not only improve the steam The heating and heat exchange efficiency reduces the preheating cost, and the indirect heat exchange of steam will not affect the alkali concentration of the slurry, so it is an efficient and energy-saving heating method; in the fifth aspect, the vanadium leaching rate guaranteed by the method can be as high as More than 90%, up to more than 97%.

申请人声明,本发明通过上述实施例来说明本发明的详细方法,但本发明并不局限于上述详细方法,即不意味着本发明必须依赖上述详细方法才能实施。所属技术领域的技术人员应该明了,对本发明的任何改进,对本发明操作的等效替换及辅助操作的添加、具体方式的选择等,均落在本发明的保护范围和公开范围之内。The applicant declares that the present invention illustrates the detailed method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed method, that is, it does not mean that the present invention must rely on the above-mentioned detailed method to be implemented. Those skilled in the art should understand that any improvement to the present invention, the equivalent replacement of the present invention's operation, the addition of auxiliary operations, the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims (10)

1. A method for double-flow feeding of a vanadium slag pressure leaching reaction kettle is characterized by comprising the following steps:
(1) mixing the first alkali liquor and the vanadium slag to obtain slurry;
(2) and (3) conveying the slurry obtained in the step (1) and the preheated second alkali liquor to a pressurized reaction kettle for oxidation leaching reaction to realize extraction of vanadium.
2. The method of claim 1, wherein the first lye of step (1) comprises NaOH solution;
preferably, the first alkali liquor in the step (1) comprises fresh alkali liquor and/or circulating alkali liquor after evaporation concentration;
preferably, the concentration of the first alkali liquor in the step (1) is 40-50 wt%;
preferably, the initial temperature of the primary alkali solution in the step (1) is 80-120 ℃.
3. The method according to claim 1 or 2, characterized in that the proportion of particles passing through a 200-mesh sieve in the vanadium slag in the step (1) is 70-90 wt%.
4. The method according to any one of claims 1 to 3, wherein the slurry of step (1) has a liquid-to-solid ratio of (1-2) to 1;
preferably, the temperature of the slurry of step (1) does not exceed 95 ℃.
5. The method of any one of claims 1-4, wherein the second alkaline solution of step (2) comprises NaOH solution;
preferably, the second alkali liquor in the step (2) comprises fresh alkali liquor and/or circulating alkali liquor after evaporation concentration;
preferably, the concentration of the second alkali liquor in the step (2) is 40-50 wt%;
preferably, the initial temperature of the second alkali liquor in the step (2) is 80-120 ℃.
6. The method according to any one of claims 1 to 5, wherein the second alkaline solution of step (2) is preheated by a pipeline preheater;
preferably, the heating medium adopted by the pipeline preheater comprises saturated steam;
preferably, the pressure of the saturated steam is not less than 2.0 MPa;
preferably, the temperature of the second alkali liquor after preheating in the step (2) is 180-220 ℃.
7. The method according to any one of claims 1 to 6, characterized in that the amount of the second alkali liquor added in the step (2) is 3 to 5 times of the mass of the vanadium slag in the step (1).
8. The method according to any one of claims 1 to 7, wherein the slurry of step (2) is delivered using a diaphragm pump;
preferably, the second alkaline solution in the step (2) is delivered by a centrifugal pump;
preferably, the impeller of the centrifugal pump is made of Ni-based alloy;
preferably, the Ni-based alloy includes any one of a Ni-Cr alloy, a Ni-Cr-Mo-Cu alloy, a Ni-Cr-Mo alloy, or a Ni-Cr-W alloy, preferably a Ni-Cr alloy.
9. The process according to any one of claims 1 to 8, wherein the pressure of the oxidative leaching reaction of step (2) is 0.6 to 1.0 MPa;
preferably, the temperature of the oxidation leaching reaction in the step (2) is 160-180 ℃;
preferably, the oxidizing gas used in the oxidizing leaching reaction in the step (2) comprises any one or a combination of at least two of oxygen, air or ozone;
preferably, the oxygen partial pressure of the oxidative leaching reaction of step (2) is 0.3-0.5 MPa.
10. Method according to any of claims 1-9, characterized in that the method comprises the steps of:
(1) mixing a first alkali solution with the initial temperature of 80-120 ℃ and the concentration of 40-50 wt% with vanadium slag with the proportion of particles passing through a 200-mesh sieve of 70-90 wt% to obtain slurry with the liquid-solid ratio (1-2): 1;
(2) preheating a second alkali solution with the initial temperature of 80-120 ℃ and the concentration of 40-50 wt% to 180-220 ℃ by adopting a pipeline preheater, wherein the heating medium is saturated steam with the pressure of not less than 2.0 MPa;
and (2) then, conveying the slurry obtained in the step (1) to a reaction kettle by using a diaphragm pump, conveying the preheated second alkali liquor to a pressurized reaction kettle by using a centrifugal pump, wherein the addition amount of the second alkali liquor is 3-5 times of the mass of the vanadium slag in the step (1), and after mixing the second alkali liquor and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.6-1.0MPa, 160-180 ℃ and 0.3-0.5MPa of oxygen partial pressure to realize extraction of vanadium.
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