CN114045400B - Method for recycling waste vanadium catalyst by column chromatography leaching - Google Patents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
- C22B34/225—Obtaining vanadium from spent catalysts
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Abstract
The invention discloses a method for recycling waste vanadium catalyst by column chromatography leaching, which comprises the steps of crushing the waste vanadium catalyst into 5-20 meshes, washing out soluble alkali metal salt in the catalyst by distilled water, concentrating and separating to obtain alkali metal salt, washing by oxalic acid solution with reduction effect, converting high-valence insoluble vanadium into soluble vanadium, placing in the solution, selectively adsorbing and separating vanadium by amino phosphoric acid chelate resin, and converting the soluble vanadium into ammonium metavanadate by ammonification and vanadium precipitation. The method has simple operation and short process, can recover the vanadium in the waste vanadium catalyst with low energy consumption and high efficiency, and can reduce the consumption of reducing agent and water.
Description
Technical Field
The invention belongs to the technical field of chemical engineering, and particularly relates to a method for recycling a waste vanadium catalyst by column chromatography leaching.
Background
In the current industrial process, vanadium is an important strategic resource, and has wide application in the fields of metal metallurgy, petrochemical industry, aviation industry, modern energy and the like due to a plurality of unique and excellent physicochemical properties. The vanadium catalyst is the key of the mass production of sulfuric acid, the poisoning failure can occur in the using process, a large amount of waste vanadium catalysts can be replaced from the device every year, if the waste vanadium catalysts are directly discarded and buried without being treated, the local soil, water sources and environment can be greatly polluted, meanwhile, a large amount of land resources can be occupied for stacking, and the vanadium belongs to a rare strategic resource and is not effectively recycled, so that the vanadium resource is seriously wasted.
At present, the processes for recycling vanadium from waste vanadium catalysts mainly comprise modes of reduction acid leaching, alkali dissolution, high-temperature roasting and the like, and high-purity vanadium pentoxide is directly or indirectly leached, enriched and converted from the waste vanadium catalysts and recovered, but the processes have the defects of complex process, high energy consumption, low efficiency, incomplete leaching of vanadium elements in leaching residues and the like.
Chinese patent CN103789550B discloses a method for recovering vanadium, potassium and silicon from waste vanadium catalyst, which comprises the following steps: firstly, carrying out pulverization, water leaching, reduction acid leaching and filtration separation on a waste vanadium catalyst, transferring alkali metal sulfate and vanadium pentoxide into a leaching solution, leaving a silicon carrier in leaching residue, and then carrying out alkali dissolution on the leaching residue to prepare sodium silicate so as to recover silicon; and extracting, back extracting, precipitating and roasting the leachate to prepare vanadium pentoxide so as to recover vanadium, and evaporating, concentrating, cooling and crystallizing the raffinate phase to prepare alkali metal sulfate so as to recover alkali metal salt. The patent scheme has the advantages of realizing the high-efficiency recovery of vanadium, silicon and potassium in the waste vanadium catalyst, and has the defects of complex process, higher cost and high energy consumption caused by the existence of steps such as evaporation concentration, roasting and the like.
The method for preparing vanadium pentoxide by treating vanadium-containing waste catalyst by two-step method of Chinese patent CN111455186A mainly comprises the following steps: crushing the waste catalyst, adding hot water and oxalic acid, stirring, soaking and filtering, adding water and concentrated sulfuric acid into filter residue obtained by filtering, soaking for the second time, adding ammonium sulfate into a leaching solution to precipitate vanadium, preparing ammonium polyvanadate, and calcining at high temperature to obtain vanadium pentoxide. The method has the problems that a large amount of water is consumed in the process of extracting vanadium, more waste water is generated, heating and stirring are needed in the leaching process, the energy consumption is high, and the leaching time long-acting rate is low.
Chinese patent CN105060344A discloses a method for extracting vanadium pentoxide from waste vanadium catalyst, which comprises the following steps: crushing and drying the waste vanadium catalyst, calcining for 2-4 h at 600-700 ℃, adding dilute ammonium bicarbonate to dissolve and filter, heating and concentrating the obtained filtrate, adding ammonium chloride to precipitate vanadium, filtering to obtain precipitate, and calcining the precipitate at high temperature to obtain vanadium pentoxide. The method also has the problems of high energy consumption and low vanadium leaching efficiency.
Disclosure of Invention
The invention aims to overcome the defects and provide the method for recovering and utilizing the waste vanadium catalyst by column chromatography leaching, which can recover vanadium in the waste vanadium catalyst with low energy consumption and high efficiency and can reduce the consumption of a reducing agent and water.
The purpose of the invention and the main technical problem of solving the invention are realized by adopting the following technical scheme:
the invention relates to a method for recovering and utilizing a waste vanadium catalyst by column chromatography leaching, which comprises the following steps:
(1) Crushing the waste vanadium catalyst to 5-20 meshes, sieving, loading the sieved waste catalyst into a chromatographic column with the diameter of 40 mm, filling the chromatographic column with the filling height of 30cm, and plugging cotton on the upper part of the chromatographic column;
(2) Pouring 300 g of distilled water slowly from the upper end of the chromatographic column, adding a liquid storage ball at the upper end of the chromatographic column after the waste catalyst particles are completely wetted, pouring 300 g of distilled water again, and collecting the leaching solution 1 at the lower end;
(3) Stopping water leaching after the catalyst in the chromatographic column turns brown, adding 10% oxalic acid solution into the liquid storage ball, and collecting leaching solution 2;
(4) Heating and boiling the leaching solution 1, filtering to obtain a suspended solid 1 and a filtrate A, continuously heating and concentrating the filtrate A until white solids are separated out, cooling and crystallizing to obtain alkali metal sulfate and a dark blue filtrate B, dissolving the solid 1 in 20 mL10% oxalic acid solution, and filtering to obtain a blue filtrate C;
(5) After all solid particles in the chromatographic column become yellow, reducing and acid leaching, mixing the leaching solution 2, the filtrate B and the filtrate C, and then selectively adsorbing and separating by using aminophosphoric acid chelate resin to obtain a blue vanadium-containing solution D;
(6) Weighing 1000 g of blue vanadium-containing solution D, heating and maintaining at 50-60 ℃, adding 50-80g of potassium perchlorate, stirring for 60min to remove the blue color of the solution, adding potassium hydroxide to adjust the pH value to be 9-10, standing and filtering to obtain filtrate E;
(7) Maintaining the temperature within the range of 50-60 ℃, adding 100-150 g of ammonium bicarbonate into the filtrate E to precipitate vanadium, stirring for 60-90 min, standing, and filtering to obtain white ammonium metavanadate solid.
The method for recycling the waste vanadium catalyst by column chromatography leaching comprises the following steps: after the reduction acid leaching in the step (5) is finished, washing yellow solid in the chromatographic column by 100g of distilled water, taking out and naturally drying to obtain SiO 2 Solid, continued to be used with the support, or converted to sodium silicate under alkaline conditions.
Compared with the prior art, the method has obvious advantages and beneficial effects, and the technical scheme shows that the method utilizes the column chromatography technology to separate and extract vanadium, firstly crushes the waste vanadium catalyst to a certain granularity, washes out soluble alkali metal salt in the catalyst by distilled water, concentrates and separates to obtain alkali metal salt, washes by oxalic acid solution with reduction effect, converts high valence state insoluble vanadium into soluble vanadium and places the soluble vanadium in the solution, then carries out selective adsorption and vanadium separation by amino phosphoric acid chelate resin, and finally converts the soluble vanadium into ammonium metavanadate through ammonification and vanadium precipitation. The separation process is simple to operate, short in process technology, low in solid-liquid ratio and low in reducing agent consumption, the whole process is completed at normal temperature and normal pressure, energy consumption is greatly reduced, sulfur oxides cannot be removed, and the separation process is environment-friendly.
Detailed Description
Example 1
A method for recovering and utilizing a waste vanadium catalyst by column chromatography leaching comprises the following steps:
(1) Crushing the waste vanadium catalyst to 5 meshes, sieving, loading the sieved waste catalyst into a chromatographic column with the diameter of 40 mm, filling the chromatographic column with the filling height of 30cm, and plugging cotton on the upper part of the chromatographic column;
(2) Pouring 300 g of distilled water slowly from the upper end of the chromatographic column to wet all the waste catalyst particles, adding a liquid storage ball at the upper end of the chromatographic column, pouring 300 g of distilled water, and collecting the leaching solution 1 at the lower end of the chromatographic column by using a 500 mL beaker;
(3) Stopping water immersion after the catalyst in the chromatographic column turns brown, adding 10% oxalic acid solution into the liquid storage ball, and simultaneously changing the beaker to continuously collect the leaching solution 2;
(4) Heating and boiling the leaching solution 1 in the beaker, filtering until suspended solids 1 and filtrate A are removed, continuously heating and concentrating the filtrate A until white solids are separated out, cooling and crystallizing to obtain alkali metal sulfate and dark blue filtrate B, dissolving the solids 1 in 20 mL10% oxalic acid solution, and filtering to obtain blue filtrate C;
(5) After the solid particles in the chromatographic column are totally yellow, reducing and acid leaching are finished, leaching solution 2, filtrate B and filtrate C are mixed, and then selective adsorption and separation are carried out by using aminophosphoric acid chelating resin to obtain blue vanadium-containing solution D;
(6) Weighing 1000 g of blue vanadium-containing solution, placing the blue vanadium-containing solution in a beaker, heating the beaker to maintain the temperature of the beaker at 50-60 ℃, adding 50 g of potassium perchlorate, stirring the solution for 60min to remove the blue color of the solution, adding potassium hydroxide to adjust the pH value of the solution to be within the range of 9-10, standing and filtering the solution to obtain filtrate E;
(7) Maintaining the temperature within the range of 50-60 ℃, adding 100g of ammonium bicarbonate into the filtrate E to precipitate vanadium, stirring for 60min, standing, and filtering to obtain an ammonium metavanadate white solid;
(8) Washing the solid particles in the chromatographic column with 100g of distilled water, and naturally drying to obtain SiO 2 The solid, which can be used as a carrier, can also be converted to potassium silicate or sodium silicate under alkaline conditions.
Through detection and analysis, the leaching rate of vanadium in the waste catalyst reaches 98.9%, the leaching rate of the alkali metal salt waste reaches 100%, the purity of ammonium metavanadate reaches 98.5%, and the recovery rate of liquid sodium silicate reaches 95.6%.
Example 2
A method for recovering and utilizing a waste vanadium catalyst by column chromatography leaching comprises the following steps:
(1) Crushing the waste vanadium catalyst to 20 meshes, sieving, loading the sieved waste catalyst into a chromatographic column with the diameter of 40 mm, filling the chromatographic column with the filling height of 30cm, and plugging cotton on the upper part of the chromatographic column;
(2) Pouring 300 g of distilled water slowly from the upper end of the chromatographic column to wet all the waste catalyst particles, adding a liquid storage ball at the upper end of the chromatographic column, pouring 300 g of distilled water, and collecting the leaching solution 1 at the lower end of the chromatographic column by using a 500 mL beaker;
(3) Stopping water immersion after the catalyst in the chromatographic column turns brown, adding 10% oxalic acid solution into the liquid storage ball, and simultaneously changing the beaker to continuously collect the leaching solution 2;
(4) Heating and boiling the leaching solution 1 in the beaker, filtering until suspended solids 1 and filtrate A are removed, continuously heating and concentrating the filtrate A until white solids are separated out, cooling and crystallizing to obtain alkali metal sulfate and dark blue filtrate B, dissolving the solids 1 in 20 mL10% oxalic acid solution, and filtering to obtain blue filtrate C;
(5) After the solid particles in the chromatographic column are totally yellow, reducing and acid leaching are finished, leaching solution 2, filtrate B and filtrate C are mixed, and then selective adsorption and separation are carried out by using aminophosphoric acid chelating resin to obtain blue vanadium-containing solution D;
(6) Weighing 1000 g of blue vanadium-containing solution, placing the blue vanadium-containing solution in a beaker, heating the beaker to maintain the temperature of the beaker at 50-60 ℃, adding 80g of potassium perchlorate, stirring the solution for 60min to remove the blue color of the solution, adding potassium hydroxide to adjust the pH value of the solution to be within the range of 9-10, standing and filtering the solution to obtain filtrate E;
(7) Maintaining the temperature within the range of 50-60 ℃, adding 150 g of ammonium bicarbonate into the filtrate E to precipitate vanadium, stirring for 90 min, standing, and filtering to obtain an ammonium metavanadate white solid;
(8) Washing the solid particles in the chromatographic column with 100g of distilled water, and naturally drying to obtain SiO 2 The solid can be used as a carrier, or can be converted into sodium silicate under alkaline conditions.
Through detection and analysis, the leaching rate of vanadium in the waste catalyst reaches 99.4%, the leaching rate of the alkali metal salt waste reaches 100%, the purity of ammonium metavanadate reaches 99.1%, and the recovery rate of liquid sodium silicate reaches 96.7%.
Example 3
A method for recovering and utilizing a waste vanadium catalyst by column chromatography leaching comprises the following steps:
(1) Crushing the waste vanadium catalyst to 10 meshes, sieving, loading the sieved waste catalyst into a chromatographic column with the diameter of 40 mm, filling the waste catalyst with the height of 30cm, and plugging cotton on the upper part of the chromatographic column;
(2) Pouring 300 g of distilled water slowly from the upper end of the chromatographic column to wet all the waste catalyst particles, adding a liquid storage ball at the upper end of the chromatographic column, pouring 300 g of distilled water, and collecting the leaching solution 1 at the lower end of the chromatographic column by using a 500 mL beaker;
(3) Stopping water immersion after the catalyst in the chromatographic column turns brown, adding 10% oxalic acid solution into the liquid storage ball, and simultaneously changing the beaker to continuously collect the leaching solution 2;
(4) Heating and boiling leaching solution 1 in a beaker, filtering until suspended solid 1 and filtrate A are removed, continuously heating and concentrating filtrate A until white solid is separated out, cooling and crystallizing to obtain alkali metal sulfate and dark blue filtrate B, dissolving solid 1 in 20 mL10% oxalic acid solution, and filtering to obtain blue filtrate C;
(5) After the solid particles in the chromatographic column are totally yellow, reducing and acid leaching are finished, leaching solution 2, filtrate B and filtrate C are mixed, and then selective adsorption and separation are carried out by using aminophosphoric acid chelating resin to obtain blue vanadium-containing solution D;
(6) Weighing 1000 g of blue vanadium-containing solution, placing the blue vanadium-containing solution in a beaker, heating the beaker to maintain the temperature of the beaker at 50-60 ℃, adding 70 g of potassium perchlorate, stirring the solution for 60min to remove the blue color of the solution, adding potassium hydroxide to adjust the pH value of the solution to be within the range of 9-10, standing and filtering the solution to obtain filtrate E;
(7) Maintaining the temperature within the range of 50-60 ℃, adding 130 g of ammonium bicarbonate into the filtrate E to precipitate vanadium, stirring for 80 min, standing, and filtering to obtain white ammonium metavanadate solid;
(8) Washing the solid particles in the chromatographic column with 100g of distilled water, and naturally drying to obtain SiO 2 The solid can be used as a carrier or can be converted into sodium silicate under alkaline conditions.
Through detection and analysis, the leaching rate of vanadium in the waste catalyst reaches 99.2%, the leaching rate of the alkali metal salt waste reaches 100%, the purity of ammonium metavanadate reaches 98.8%, and the recovery rate of liquid sodium silicate reaches 96.4%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the present invention without departing from the technical spirit of the present invention.
Claims (2)
1. A method for recovering and utilizing a waste vanadium catalyst by column chromatography leaching comprises the following steps:
(1) Crushing the waste vanadium catalyst to 5-20 meshes, sieving, loading 30 g of the sieved waste catalyst into a chromatographic column with the diameter of 40 mm, filling the waste catalyst with the height of 30cm, and plugging cotton on the upper part of the chromatographic column;
(2) Pouring 300 g of distilled water slowly from the upper end of the chromatographic column to wet all the waste catalyst particles, adding a liquid storage ball at the upper end of the chromatographic column, pouring 300 g of distilled water, and collecting the leaching solution 1 at the lower end;
(3) Stopping water immersion after the catalyst in the chromatographic column turns brown, adding 10% oxalic acid solution into the liquid storage ball, and collecting an extract 2;
(4) Heating the leaching solution 1 to boil, filtering to obtain a suspended solid 1 and a filtrate A, continuously heating and concentrating the filtrate A until white solids are separated out, cooling and crystallizing to obtain an alkali metal sulfate and a dark blue filtrate B, dissolving the solid 1 in 20 mL10% oxalic acid solution, and filtering to obtain a blue filtrate C;
(5) After the solid particles in the chromatographic column are totally yellow, reducing and acid leaching are finished, leaching solution 2, filtrate B and filtrate C are mixed, and then selective adsorption and separation are carried out by using aminophosphoric acid chelating resin to obtain blue vanadium-containing solution D;
(6) Weighing 1000 g of blue vanadium-containing solution D, heating and maintaining at 50-60 ℃, adding 50-80g of potassium perchlorate, stirring for 60min to remove the blue color of the solution, adding potassium hydroxide to adjust the pH value to be 9-10, standing and filtering to obtain filtrate E;
(7) Maintaining the temperature within the range of 50-60 ℃, adding 100-150 g of ammonium bicarbonate into the filtrate E to precipitate vanadium, stirring for 60-90 min, standing, and filtering to obtain white ammonium metavanadate solid.
2. The method of claim 1A method for recovering and utilizing a waste vanadium catalyst by column chromatography leaching, which comprises the following steps: after the reduction acid leaching in the step (5) is finished, washing yellow solid in the chromatographic column by 100g of distilled water, taking out and naturally drying to obtain SiO 2 Solid, used as a carrier, or converted to sodium silicate under alkaline conditions.
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