CN114318014B - Method for double-flow feeding of vanadium slag pressure leaching reaction kettle - Google Patents
Method for double-flow feeding of vanadium slag pressure leaching reaction kettle Download PDFInfo
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- CN114318014B CN114318014B CN202111624946.1A CN202111624946A CN114318014B CN 114318014 B CN114318014 B CN 114318014B CN 202111624946 A CN202111624946 A CN 202111624946A CN 114318014 B CN114318014 B CN 114318014B
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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
Technical Field
The invention belongs to the technical field of vanadium chemical metallurgy, and particularly relates to a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle.
Background
The vanadium slag is a vanadium-enriched material blown from vanadium-containing molten iron in the presence of oxygen-containing gas, and the vanadium slag produced from vanadium-titanium magnetite in the steel industry is a main raw material for extracting vanadium. Enterprises which produce iron and vanadium products by taking vanadium titano-magnetite as a raw material adopt the traditional vanadium slag sodium salt roasting process to extract vanadium from vanadium slag, such as Pan steel and bearing steel in China, south Africa Hai Weird, new Zealand steel companies and the like. The basic principle of the sodium roasting process is Na 2 CO 3 As an additive, low-valence vanadium is converted into water-soluble sodium salt of pentavalent vanadium by high-temperature sodium salt roasting (750-850 ℃), then the sodium salt roasting product is directly soaked in water to obtain vanadium-containing leaching solution, ammonium salt is added to prepare ammonium polyvanadate precipitate, and the vanadium oxide product is obtained by reduction roasting. However, the recovery rate of vanadium in the sodium roasting process is low, the recovery rate of vanadium in single roasting is about 70%, and the recovery rate of vanadium after multiple roasting is only 80%; the roasting temperature is high (750-850 ℃), and multiple times of roasting are needed, so that the energy consumption is high; after being roastedIn the process, harmful HCl and Cl are also generated 2 And the like, and pollute the environment. Therefore, the vanadium extraction process from the vanadium slag, which has the advantages of low energy consumption, simple process flow, safety and environmental protection, has important significance.
CN102531056A discloses a method for a vanadium slag pressure leaching pressure reactor, which comprises the steps of firstly stirring and mixing a NaOH solution and vanadium slag in a preparation tank to prepare slurry with a liquid-solid ratio of 4-6:1, and then conveying all the slurry to the pressure reactor through an alkali-resistant, high-temperature-resistant and wear-resistant pump to perform leaching reaction. However, the method has high requirements on equipment, the corrosion and abrasion of the equipment are serious, the feeding is carried out by adopting a single feeding pump, the feeding time is long, a heating device is required to be added in the pressurized reaction kettle, the cost of the equipment is increased, the whole reaction period is prolonged, and the energy consumption is high.
CN110760687A discloses a method for low-cost clean vanadium extraction from vanadium slag, which comprises four steps of vanadium slag roasting, alkaline leaching, purification and vanadium precipitation, wherein the vanadium slag is roasted after being mixed with calcium oxide to obtain roasted clinker, the roasted clinker is subjected to alkaline leaching to obtain residue and vanadium-containing leachate, washing liquor after residue washing is concentrated and mixed with the vanadium-containing leachate to obtain vanadium-containing mixed liquor, the vanadium-containing mixed liquor and calcium chloride are obtained to obtain sodium vanadate solution, the sodium vanadate solution is added with ammonium chloride solution for solid-liquid separation to obtain ammonium metavanadate precipitate and vanadium precipitation wastewater, and the vanadium precipitation wastewater is returned to the alkaline leaching step for alkaline leaching of the roasted clinker. The method adopts a sodium treatment roasting process, but the method adopts the mixed roasting with calcium oxide, but the roasting temperature is also higher, and the energy consumption is higher.
In conclusion, how to provide a vanadium extraction process from vanadium slag, which has the advantages of low energy consumption, simple process flow, safety and environmental protection, becomes a problem to be solved urgently at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which adopts a double-flow feeding mode, greatly reduces the loss of slurry to equipment, is efficient and environment-friendly, and is suitable for industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
(1) Mixing the first alkali liquor and the vanadium slag to obtain slurry;
(2) And (2) 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.
In the invention, the first alkali liquor and the second alkali liquor can be divided into two parts by the same alkali liquor, and can also be prepared respectively and independently.
According to the invention, the traditional method of mixing materials firstly and then feeding is optimized, the alkali liquor is divided, one part of the alkali liquor and the vanadium slag form slurry, and the other part of the alkali liquor and the formed slurry are fed in a double-flow mode.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical scheme of the invention, the first alkali liquor in the step (1) comprises NaOH solution.
Preferably, the first alkali liquor in step (1) comprises fresh alkali liquor and/or circulating alkali liquor after evaporation concentration.
Preferably, the concentration of the first lye of step (1) is in the range of 40 to 50 wt.%, such as 40 wt.%, 41 wt.%, 42 wt.%, 43 wt.%, 44 wt.%, 45 wt.%, 46 wt.%, 47 wt.%, 48 wt.%, 49 wt.% or 50 wt.%, etc., but is not limited to the recited values, and other non-recited values within this range are equally applicable.
Preferably, the initial temperature of the primary alkali solution in step (1) is 80-120 deg.C, such as 80 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, 115 deg.C or 120 deg.C, but not limited to the recited values, and other unrecited values within the range of values are equally applicable.
In a preferred embodiment of the present invention, the ratio of the particles passing through the 200 mesh sieve in the vanadium slag in step (1) is 70-90wt%, for example, 70wt%, 72wt%, 74wt%, 76wt%, 78wt%, 80wt%, 82wt%, 84wt%, 86wt%, 88wt%, or 90wt%, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
As a preferred embodiment of the present invention, the slurry in step (1) has a liquid-solid ratio of (1.0-2) 1, for example, 1.0.
Preferably, the temperature of the slurry in step (1) does not exceed 95 ℃, such as 80 ℃, 82 ℃, 84 ℃, 86 ℃, 88 ℃, 90 ℃, 93 ℃ or 95 ℃, but is not limited to the recited values, and other unrecited values within the range of values are equally applicable.
In the invention, the slurry in the step (2) is conveyed by adopting the diaphragm pump, and because the diaphragm pump has no shaft seal, no leakage, wide flow passage, no impeller and small abrasion of parts of the pump, when the slurry contains particles, and volatile and corrosive media are conveyed, the slurry cannot cause environmental pollution and harm the personal safety. However, the diaphragm pump has requirements on the feeding temperature, and the feeding temperature is not higher than 95 ℃, so that the liquid-solid ratio of the slurry is very important, and the method controls the temperature of the slurry by adjusting the liquid-solid ratio. If the liquid-solid ratio is too large, the temperature of the slurry is too high, and the corrosion of the diaphragm pump is aggravated when the temperature exceeds 95 ℃, so that the service life is influenced; if the liquid-solid ratio is too low, the solid content of the slurry is too high, the slurry cannot be normally conveyed, and a feeding pipeline is easily blocked.
As a preferred technical solution of the present invention, the second alkaline solution in step (2) includes NaOH solution.
Preferably, the second alkali liquor in step (2) comprises fresh alkali liquor and/or circulating alkali liquor after evaporation concentration.
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%, 49wt% or 50wt%, etc., but not limited to the recited values, and other non-recited values in the range of the values are also applicable.
Preferably, the initial temperature of the second alkali solution in step (2) is 80-120 deg.C, such as 80 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, 115 deg.C or 120 deg.C, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
As a preferable technical scheme of the invention, the second alkali liquor in the step (2) is preheated by a pipeline preheater.
Preferably, the heating medium used by the tube preheater comprises saturated steam.
Preferably, the pressure of the saturated steam is not less than 2.0MPa, such as 2.0MPa, 2.2MPa, 2.3MPa, 2.5MPa, 3.0MPa, 3.2MPa, 3.5MPa, 3.8MPa, or 4.0MPa, but is not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the temperature of the second alkaline solution after preheating in step (2) is 180-220 ℃, such as 180 ℃, 185 ℃, 190 ℃, 195 ℃, 200 ℃, 205 ℃, 210 ℃, 215 ℃ or 220 ℃, but not limited to the recited values, and other unrecited values in the range of the values are also applicable.
In the invention, the traditional pressure oxidation reaction adopts direct steam heating or electromagnetic induction heating, and the direct steam heating can cause the alkali liquor slurry in the reaction kettle to be diluted, thereby influencing the extraction effect of vanadium; electromagnetic induction heating is then through heating the reation kettle cauldron body, and the cauldron body is with heat transfer for thick liquids again, and the cauldron body heat dissipation is big, the thermal efficiency is low, and the energy consumption cost of electrical heating is higher than steam moreover. The steam pipeline preheating of the invention can not only improve the steam heating heat exchange efficiency and reduce the preheating cost, but also can not influence the alkali concentration of the slurry through the indirect steam heat exchange, thus being a high-efficiency and energy-saving heating method.
In a preferred embodiment of the present invention, the amount of the second alkaline solution added in step (2) is 3 to 5 times, for example, 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 the mass of the vanadium slag in step (1), but is not limited to the above-mentioned values, and other values not listed in the above-mentioned value range are also applicable.
As a preferable technical scheme of the invention, the slurry in the step (2) is conveyed by a diaphragm pump.
Preferably, the second alkaline solution in the step (2) is delivered by using 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 (W) alloy, or a Ni-Cr-W alloy, preferably a Ni-Cr alloy.
In a preferred embodiment of the present invention, the pressure of the oxidative leaching reaction in the step (2) is 0.6 to 1.0MPa, for example, 0.60MPa, 0.65MPa, 0.70MPa, 0.75MPa, 0.80MPa, 0.85MPa, 0.90MPa, 0.95MPa or 1.00MPa, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the temperature of the oxidative leaching reaction in step (2) is 160-180 ℃, such as 160 ℃, 163 ℃, 166 ℃, 169 ℃, 172 ℃, 175 ℃, 178 ℃ or 180 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In the invention, the temperature of the preheated second alkali liquor and the slurry can reach the set reaction temperature of 160-180 ℃ after mixing, heating equipment is not required to be added to the reaction kettle, and the leaching temperature can be ensured by the reaction heat release in the oxidation leaching process, so that the energy consumption is saved, and the equipment investment of the reaction kettle is reduced.
Preferably, the oxidizing gas used in the oxidizing leaching reaction in step (2) comprises any one of oxygen, air or ozone or a combination of at least two of oxygen, air and ozone.
Preferably, the oxygen partial pressure of the oxidative leaching reaction in step (2) is 0.3 to 0.5MPa, such as 0.30MPa, 0.33MPa, 0.36MPa, 0.39MPa, 0.42MPa, 0.45MPa, 0.48MPa, or 0.50MPa, but not limited to the recited values, and other values not recited in this range are also applicable.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) Mixing a first alkali solution with the initial temperature of 80-120 ℃ and the concentration of 40-50wt% with vanadium slag with the proportion of particles passing through a 200-mesh sieve of 70-90wt% to obtain slurry with the liquid-solid ratio (1-2): 1;
(2) Preheating the second alkali liquor 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) into a reaction kettle by using a diaphragm pump, conveying a preheated second alkali liquor into 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.
Compared with the prior art, the invention has the following beneficial effects:
(1) The vanadium slag pressure leaching reaction kettle double-flow feeding method optimizes the traditional method of firstly mixing and then feeding, mixes part of alkali liquor and vanadium slag to form slurry, and then realizes double-flow feeding of the other part of alkali liquor and the obtained slurry, so that the feeding process is simpler and more efficient;
(2) The method controls the temperature of the slurry to be not more than 95 ℃ by preparing the vanadium slag slurry with low liquid-solid ratio, thereby meeting the requirement of a diaphragm pump on the material conveying temperature and ensuring that the vanadium slag slurry can adopt a durable diaphragm pump as a feeding pump of a pressurization reaction kettle;
(3) According to the method, the diaphragm pump is used for conveying the slurry into the reaction kettle, so that the loss of the slurry to the impeller of the traditional conveying pump can be avoided, and the service cycle of equipment is prolonged;
(4) The method adopts a pipeline preheating mode to preheat the second alkali liquor to the reaction temperature, and as the liquid alkali does not contain solid particles, the abrasion of a pump impeller for conveying the alkali liquor is greatly reduced, and the service life of the pump impeller can be obviously prolonged;
(5) The second alkali liquor in the method is heated by adopting a steam pipelining preheating method, so that the steam heating heat exchange efficiency can be improved, the preheating cost is reduced, the indirect heat exchange of the steam cannot influence the alkali concentration of the slurry, and the method is an efficient and energy-saving heating method;
(6) The method of the invention can lead the recovery rate of vanadium to reach more than 90 percent and reach more than 97 percent at most.
Drawings
FIG. 1 is a process flow diagram of a double-flow feeding method of a vanadium slag pressure leaching reaction kettle provided in embodiment 1 of the invention.
Detailed Description
In order to better explain the present invention and to facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a method for performing pressure leaching on vanadium slag by using a double-flow feeding of a reaction kettle, and the process flow of the method is shown in figure 1.
The method comprises the following steps:
providing an evaporated circulating NaOH solution with the initial temperature of 90 ℃ and the concentration of 45wt%, and dividing the circulating NaOH solution into an A strand and a B strand, wherein the A strand is a first NaOH solution, and the B strand is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 80wt% of particles to obtain slurry with a liquid-solid ratio of 1.6;
(2) Preheating the second NaOH solution to 180 ℃ by adopting a pipeline preheater, wherein the heating medium is saturated steam with the pressure of 3.0 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr alloy, wherein the addition amount of the second NaOH solution is 3.4 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.8MPa, 160 ℃ and 0.4MPa of oxygen partial pressure to realize extraction of vanadium.
Example 2:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing a freshly prepared NaOH solution with the initial temperature of 86 ℃ and the concentration of 48wt%, and dividing the freshly prepared NaOH solution into an A strand and a B strand, wherein the A strand is a first NaOH solution, and the B strand is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 84wt% of particle ratio to obtain slurry with the liquid-solid ratio of 2.0;
(2) Preheating the second NaOH solution to 210 ℃ by adopting a pipeline preheater, wherein the heating medium is saturated steam with the pressure of 3.6 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by adopting a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by utilizing a centrifugal pump with an impeller made of Ni-Cr alloy, wherein the addition amount of the second NaOH solution is 3.0 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.8MPa, 175 ℃ and 0.45MPa of oxygen partial pressure to realize extraction of vanadium.
Example 3:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing an evaporated circulating NaOH solution with the initial temperature of 80 ℃ and the concentration of 50wt%, and dividing the circulating NaOH solution into an A strand and a B strand, wherein the A strand is a first NaOH solution, and the B strand is a second NaOH solution;
(1) Mixing the first NaOH solution with 86wt% vanadium slag which is sieved by a 200-mesh sieve to obtain slurry with a liquid-solid ratio of 1.8;
(2) Preheating the second NaOH solution to 220 ℃ by adopting a pipeline preheater, wherein a heating medium is saturated steam with the pressure of 3.7 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr-Mo-Cu alloy, wherein the addition amount of the second NaOH solution is 3.2 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.8MPa, 180 ℃ and 0.50MPa of oxygen partial pressure to realize extraction of vanadium.
Example 4:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing a freshly prepared NaOH solution with the initial temperature of 88 ℃ and the concentration of 48wt%, and dividing the freshly prepared NaOH solution into a strand A and a strand B, wherein the strand A is a first NaOH solution, and the strand B is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 76wt% of particles to obtain slurry with a liquid-solid ratio of 1.0;
(2) Preheating the second NaOH solution to 215 ℃ by adopting a pipeline preheater, wherein the heating medium is saturated steam with the pressure of 3.0 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr alloy, wherein the addition amount of the second NaOH solution is 4.0 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.9MPa, 178 ℃ and 0.40MPa of oxygen partial pressure to realize extraction of vanadium.
Example 5:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing an evaporated circulating NaOH solution with the initial temperature of 110 ℃ and the concentration of 47wt%, and dividing the circulating NaOH solution into a strand A and a strand B, wherein the strand A is a first NaOH solution, and the strand B is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 70wt% of particles to obtain slurry with a liquid-solid ratio of 1.4;
(2) Preheating the second NaOH solution to 200 ℃ by adopting a pipeline preheater, wherein the heating medium is saturated steam with the pressure of 2.0 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr alloy, wherein the addition amount of the second NaOH solution is 3.6 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.92MPa, 170 ℃ and 0.38MPa of oxygen partial pressure to realize extraction of vanadium.
Example 6:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing an evaporated circulating NaOH solution with the initial temperature of 105 ℃ and the concentration of 48wt%, and dividing the circulating NaOH solution into a strand A and a strand B, wherein the strand A is a first NaOH solution, and the strand B is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 88wt% of particles to obtain slurry with a liquid-solid ratio of 1.5;
(2) Preheating the second NaOH solution to 190 ℃ by adopting a pipeline preheater, wherein a heating medium is saturated steam with the pressure of 3.2 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr alloy, wherein the addition amount of the second NaOH solution is 3.5 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.95MPa, 165 ℃ and 0.35MPa of oxygen partial pressure to realize extraction of vanadium.
Example 7:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing an evaporated circulating NaOH solution with the initial temperature of 90 ℃ and the concentration of 46wt%, and dividing the circulating NaOH solution into an A strand and a B strand, wherein the A strand is a first NaOH solution, and the B strand is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 72wt% of particles to obtain slurry with a liquid-solid ratio of 1.3;
(2) Preheating the second NaOH solution to 185 ℃ by adopting a pipeline preheater, wherein the heating medium is saturated steam with the pressure of 2.5 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr-Mo alloy, wherein the addition amount of the second NaOH solution is 3.7 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.75MPa, 163 ℃ and 0.30MPa of oxygen partial pressure to realize extraction of vanadium.
Example 8:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing an evaporated circulating NaOH solution with the initial temperature of 120 ℃ and the concentration of 50wt%, and dividing the circulating NaOH solution into a strand A and a strand B, wherein the strand A is a first NaOH solution, and the strand B is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 90wt% of particles to obtain slurry with a liquid-solid ratio of 1.0;
(2) Preheating the second NaOH solution to 220 ℃ by adopting a pipeline preheater, wherein the heating medium is saturated steam with the pressure of 4.0 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr alloy, wherein the addition amount of the second NaOH solution is 4.0 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 1.0MPa, 180 ℃ and 0.5MPa of oxygen partial pressure to realize extraction of vanadium.
Example 9:
the embodiment provides a method for double-flow feeding of a vanadium slag pressure leaching reaction kettle, which comprises the following steps:
providing an evaporated circulating NaOH solution with the initial temperature of 80 ℃ and the concentration of 45wt%, and dividing the circulating NaOH solution into an A strand and a B strand, wherein the A strand is a first NaOH solution, and the B strand is a second NaOH solution;
(1) Mixing the first NaOH solution with vanadium slag which is sieved by a 200-mesh sieve and has 74wt% of particles to obtain slurry with a liquid-solid ratio of 1.9;
(2) Preheating the second NaOH solution to 180 ℃ by adopting a pipeline preheater, wherein a heating medium is saturated steam with the pressure of 3.5 MPa;
and (2) then, conveying the slurry obtained in the step (1) into a reaction kettle by using a diaphragm pump, conveying a preheated second NaOH solution into a pressurized reaction kettle by using a centrifugal pump with an impeller made of Ni-Cr alloy, wherein the addition amount of the second NaOH solution is 3.1 times of the mass of the vanadium slag obtained in the step (1), and after mixing the second NaOH solution and the vanadium slag, carrying out oxidation leaching reaction under the conditions of 0.60MPa, 160 ℃ and 0.30MPa of oxygen partial pressure to realize extraction of vanadium.
Example 10:
this example provides a method of pressure leaching of vanadium slag with dual feed to the autoclave, which is referred to the method of example 4, except that: the liquid-solid ratio of the slurry obtained in the step (1) is 0.5.
Example 11:
this example provides a method of pressure leaching of vanadium slag with dual feed to the autoclave, which is referred to the method of example 2, except that: the liquid-solid ratio of the slurry obtained in the step (1) is 2.5.
Example 12:
this example provides a method of pressure leaching of vanadium slag with dual feed to the autoclave, which is referred to the method of example 1, except that: and (3) the impeller of the centrifugal pump in the step (2) is made of 316L stainless steel.
The leaching rates of vanadium in examples 1 to 12 were measured, and the results are shown in Table 1.
TABLE 1
Examples 1-9 adopt the method of the invention, through optimizing the feeding way, have guaranteed the leaching rate of vanadium while improving the apparatus service life, make it reach more than 90%, can reach more than 97% at most; in the embodiment 10, the solid-to-solid ratio of the slurry formed by mixing the first alkali liquor and the vanadium slag is too small, so that the slurry is very difficult to convey, and the blockage frequency of a feed pipeline is very high; in the embodiment 11, the solid-to-solid ratio of the slurry formed by mixing the first alkali liquor and the vanadium slag is too high, so that the temperature of the slurry reaches 110 ℃, and the service life of a rubber diaphragm in the diaphragm pump is shortened from one year to 3 months; in example 12, the impeller of the centrifugal pump for delivering the second alkali solution is made of conventional 316L stainless steel, and although the leaching rate of vanadium is not affected, the service life of the impeller of the centrifugal pump is shortened from 6 months to 2 months, thereby increasing the equipment cost.
It can be seen from the above embodiments that, in the first aspect, the dual-flow feeding method for the vanadium slag pressure leaching reaction kettle optimizes the traditional method of first proportioning and then feeding, mixes part of the alkali liquor with the vanadium slag to form slurry, and then feeds the other part of the alkali liquor and the obtained slurry in a dual-flow manner, so that the feeding process is simpler and more efficient; in the second aspect, the method controls the temperature of the slurry to be not more than 95 ℃ by preparing the vanadium slag slurry with low liquid-solid ratio, thereby meeting the requirement of a diaphragm pump on the material conveying temperature and ensuring that the vanadium slag slurry can adopt a durable diaphragm pump as a feeding pump of a pressurized reaction kettle; in the third aspect, the method utilizes the diaphragm pump to convey the slurry into the reaction kettle, so that the loss of the slurry to a traditional conveying pump impeller can be avoided, and the service life of equipment is prolonged; in the fourth aspect, the second alkali liquor in the method is heated by adopting a steam pipelining preheating method, so that the steam heating heat exchange efficiency can be improved, the preheating cost can be reduced, the indirect heat exchange of the steam cannot influence the alkali concentration of the slurry, and the method is an efficient and energy-saving heating method; in the fifth aspect, the leaching rate of vanadium guaranteed by the method can reach more than 90 percent, and can reach more than 97 percent at most.
The applicant states that the present invention is illustrated by the above examples to show the detailed method of the present invention, but the present invention is not limited to the above detailed method, that is, it does not mean that the present invention must rely on the above detailed method to be carried out. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
Claims (24)
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;
the liquid-solid ratio of the slurry in the step (1) is (1-2) to 1;
the temperature of the slurry in the step (1) is not more than 95 ℃;
(2) 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 adding amount of the second alkali liquor in the step (2) is 3-5 times of the mass of the vanadium slag in the step (1).
2. The method of claim 1, wherein step (1) said primary alkali solution comprises NaOH solution.
3. The method according to claim 1, wherein the first lye of step (1) comprises fresh lye and/or recycled lye after concentration by evaporation.
4. The method as claimed in claim 1, wherein the concentration of the primary alkali solution in step (1) is 40-50wt%.
5. The method as claimed in claim 1, wherein the initial temperature of the primary alkali solution in step (1) is 80-120 ℃.
6. The method according to claim 1, characterized in that the proportion of the particles passing through the 200-mesh sieve in the vanadium slag in the step (1) is 70-90wt%.
7. The method of claim 1, wherein the second alkaline solution of step (2) comprises a NaOH solution.
8. The method according to claim 1, wherein the second alkaline solution in step (2) comprises a fresh alkaline solution and/or a recycled alkaline solution after evaporation concentration.
9. The method as claimed in claim 1, wherein the concentration of the second alkali solution in step (2) is 40-50wt%.
10. The method as claimed in claim 1, wherein the initial temperature of the secondary alkali solution in step (2) is 80-120 ℃.
11. The method of claim 1, wherein the second alkaline solution of step (2) is preheated using a tube preheater.
12. The method of claim 11, wherein the heating medium employed by the tube preheater comprises saturated steam.
13. The method of claim 12, wherein the saturated steam has a pressure of not less than 2.0MPa.
14. The method of claim 1, wherein the temperature of the second alkaline solution after preheating in step (2) is 180-220 ℃.
15. The method of claim 1, wherein the slurry of step (2) is delivered using a diaphragm pump.
16. The method of claim 1, wherein the second caustic of step (2) is delivered using a centrifugal pump.
17. The method of claim 16 wherein the impeller material of the centrifugal pump comprises a Ni-based alloy.
18. The method of claim 17, wherein the Ni-based alloy comprises any one of a Ni-Cr alloy, a Ni-Cr-Mo-Cu alloy, a Ni-Cr-Mo alloy, or a Ni-Cr-W alloy.
19. The method of claim 18, wherein the Ni-based alloy is a Ni-Cr alloy.
20. The method according to claim 1, wherein the pressure of the oxidative leaching reaction of step (2) is 0.6-1.0MPa.
21. The method of claim 1, wherein the temperature of the oxidative leaching reaction of step (2) is 160-180 ℃.
22. The method of claim 1, wherein the oxidizing gas used in the oxidizing leaching reaction of step (2) comprises any one of oxygen, air or ozone or a combination of at least two of oxygen, air and ozone.
23. The method according to claim 1, wherein the oxygen partial pressure of the oxidative leaching reaction of step (2) is 0.3-0.5MPa.
24. Method according to claim 1, characterized in that it comprises the following steps:
(1) Mixing a first alkali solution with the initial temperature of 80-120 ℃ and the concentration of 40-50wt% with vanadium slag with the proportion of particles passing through a 200-mesh sieve of 70-90wt% to obtain slurry with the liquid-solid ratio (1-2): 1;
(2) Preheating a second alkali liquor with the initial temperature of 80-120 ℃ and the concentration of 40-50wt% to 180-220 ℃ by adopting a pipeline preheater, wherein a 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) into a reaction kettle by using a diaphragm pump, conveying a preheated second alkali liquor into 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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| US4443415A (en) * | 1982-06-22 | 1984-04-17 | Amax Inc. | Recovery of V2 O5 and nickel values from petroleum coke |
| US4666685A (en) * | 1986-05-09 | 1987-05-19 | Amax Inc. | Selective extraction of molybdenum and vanadium from spent catalysts by oxidative leaching with sodium aluminate and caustic |
| CN201144225Y (en) * | 2007-11-05 | 2008-11-05 | 李大光 | Reactor for processing waste tyre and waste plastic using cracking method |
| CN102531056B (en) * | 2012-01-09 | 2014-11-05 | 中国科学院过程工程研究所 | Method for cleaner production of sodium vanadate and sodium chromate by pressure leaching of vanadium slag |
| CN105400967B (en) * | 2015-11-10 | 2018-07-03 | 中国科学院过程工程研究所 | A kind of method of low-temperature atmosphere-pressure extraction Vanadium in Vanadium Residue and chromium |
| EP3214190A1 (en) * | 2016-03-01 | 2017-09-06 | SMS Siemag Process Technologies GmbH | Process for the separation of vanadium |
| CN108298581B (en) * | 2017-01-11 | 2021-03-30 | 中国科学院过程工程研究所 | System for extracting vanadium from leaching solution containing vanadium, chromium and silicon and preparing vanadium pentoxide and treatment method thereof |
| CN107236866B (en) * | 2017-06-22 | 2020-04-03 | 中国科学院过程工程研究所 | Method for pressure strengthening vanadium extraction from vanadium-containing steel slag |
| CN107236871B (en) * | 2017-06-22 | 2020-04-17 | 河钢股份有限公司承德分公司 | Method for extracting vanadium from mixed vanadium slag and vanadium-containing steel slag under pressure |
| CN108658126A (en) * | 2018-06-29 | 2018-10-16 | 河钢股份有限公司承德分公司 | A method of extracting vanadium from calcium phosphorus slag |
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