CN110923459A - Method for recovering titanium-tungsten powder from waste SCR catalyst - Google Patents
Method for recovering titanium-tungsten powder from waste SCR catalyst Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- 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
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
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- C—CHEMISTRY; METALLURGY
- 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
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
- C22B34/365—Obtaining tungsten from spent catalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for recovering titanium tungsten powder from a waste SCR catalyst, which comprises the steps of grinding the waste SCR catalyst and then screening to obtain waste catalyst powder with the granularity of less than 5 mu m; and then adding oxalic acid leaching, hydrofluoric acid leaching and sulfuric acid solution acid leaching in three steps respectively, removing arsenic oxide and silicon dioxide, finally filtering to obtain a titanium sulfate solution, adding a surfactant, precipitating with ammonia water, removing impurities together with filter residue to remove Fe, K and Na, calcining at high temperature, and grinding to obtain titanium-tungsten powder. The method has simple process, the recovery rate of vanadium is more than 99 percent, the recovery rates of titanium and tungsten are more than 95 percent, the recovery rate of silicon dioxide is less than 0.5 percent, and the specific surface area of the recovered titanium-tungsten powder is 90m higher2More than g, pore volume greater than 0.3cm3Per g, impuritiesThe mass Fe, K, Na and As is less than 100ug/g, and the index requirement of the industrial denitration catalyst for producing titanium tungsten powder is completely met.
Description
Technical Field
The invention relates to a method for recovering a catalyst, in particular to a method for recovering titanium-tungsten powder from a waste SCR catalyst.
Background
Most of domestic coal-fired power plants and other boilers mainly use coal as fuel, generate more nitrogen oxides in the combustion process, predict that the generation amount is about 240.5 ten thousand tons in 2020, have great harm to environmental pollution, and must be removedNitrogen oxides. At present, the industrial denitration catalyst is mainly a medium-high temperature catalyst, mainly V-W (Mo)/TiO2In the denitration reaction process, trace alkali metal, sulfur, arsenic, mercury and other substances in the flue gas are deposited or react with active substances, so that the SCR catalyst is quickly deactivated, and finally the catalyst cannot be replaced when the emission requirement is met. The catalyst contains metals such as Ti, W, V and the like, and the waste catalyst rich in metals is not used, so that not only is resources wasted, but also the environment is polluted, and the state brings the waste flue gas denitration catalyst (vanadium-titanium series) into HW50 in hazardous waste.
Patent CN103484678A discloses a method for recovering vanadium, tungsten and titanium from waste vanadium tungsten titanium-based denitration catalyst, mixing the crushed waste catalyst with concentrated alkali solution, heating to react to generate slightly soluble titanate and water-soluble vanadate and tungstate, after solid-liquid separation, adding ammonium metavanadate and concentrated acid to generate ammonium metavanadate and extracting tungstic acid respectively. Wherein, the recovery rate of vanadium is more than 90 percent, the recovery rate of tungsten is more than 80 percent, and the recovery rate of titanium is more than 80 percent. The method has the advantages of complex operation, lower yield, high temperature of 120 ℃ and 350 ℃ and higher energy consumption, and the pH value of the solution needs to be strictly controlled in the chemical reaction process.
The method for preparing titanium-tungsten powder by recovering the waste SCR denitration catalyst with the patent number of 201811257800.6 comprises the steps of pretreating waste catalyst powder by using sulfuric acid activation treatment, and then removing glass fibers in coarse activation slurry to obtain purified activation slurry; heating, purifying and activating the slurry to obtain reconstructed slurry; filtering the reconstructed slurry to obtain a solid-phase product and a filtrate; and washing, drying and calcining the solid-phase product to obtain the titanium-tungsten powder product. In the method, the removal of the glass fiber in the catalyst by using sulfuric acid activation treatment is limited, the glass fiber and the catalyst mud are melted into a whole during high-temperature calcination in the production process of the denitration catalyst, the separation is difficult, and the recovery and the utilization of tungsten trioxide are low.
The recovery method for comprehensively analyzing titanium tungsten powder in the waste denitration catalyst adopts alkaline leaching in the prior art, has long leaching time and large alkaline consumption, and particularly obtains titanium dioxide by acidification in the later period; the recovery rate of vanadium and tungsten is low, and the cost is greatly increased. Another method uses acidification to strip the glass fibers and has limited implementation. Therefore, further research and exploration is needed for other methods of titanium tungsten powder recovery to achieve effective methods at lower cost.
Disclosure of Invention
The invention aims to provide a method for recovering titanium-tungsten powder from a waste SCR catalyst, so as to solve the technical problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a method for recovering titanium tungsten powder from a waste SCR catalyst comprises the following steps:
s1: grinding the waste SCR catalyst and then screening to obtain waste catalyst powder with the granularity less than 5 mu m;
s2: adding oxalic acid with the concentration of 20% -30% into the waste catalyst powder obtained in the step S1 for acid leaching, filtering to obtain a vanadium oxalate solution, evaporating, crystallizing and filtering to obtain a vanadium oxalate product, wherein the leaching temperature is 85-95 ℃, and the leaching end point is that the total content of vanadium in filter residue is less than 0.01%;
s3: adding 0.5-1 mol/L hydrofluoric acid into the filter residue in the S2 for acid leaching, wherein the leaching temperature is 80-90 ℃, the adding amount of the hydrofluoric acid is 1.05-1.1 times of the theoretical required amount of silicon, the reaction time is 1.0-1.5h, the end point of the leaching is that the total amount of the metal silicon in the filter residue is less than 0.5 percent, recovering the gaseous silicon fluoride, adding ethanol, and cleaning to remove arsenic until the content of the arsenic is less than 100 ug/g;
s4: and adding 50-60% sulfuric acid solution into the filter residue in the S3 for acid leaching, wherein the leaching temperature is 120-180 ℃, the reaction end point is that the total titanium content in the filter residue is less than 0.1%, filtering to obtain titanium sulfate solution, adding a surfactant, precipitating with ammonia water, removing impurities together with the filter residue to remove Fe, K and Na, calcining at high temperature, and grinding to obtain titanium-tungsten powder.
As a preferable technical scheme of the invention, the oxalic acid is added in the step S2 in a vanadium molar ratio of 1:2-1:5, and the reaction time is 2.0-3.0 h.
As a preferable technical scheme of the invention, the adding amount of the sulfuric acid in the step S4 is 1.1-1.2 times of the theoretical required amount of the titanium, and the reaction time is 3.5-5.0 h.
In a preferred embodiment of the present invention, in step S4, the surfactant is any one of (polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer) P123, cetyltrimethylammonium hydroxide, and primary amine, and the amount of the surfactant added is 0.1% to 0.3% of the amount of the solution.
As a preferable technical scheme of the invention, the temperature of the high-temperature calcination in the step S4 is 400-550 ℃, and the calcination time is 4-6 h.
In a preferred embodiment of the present invention, the titanium-tungsten powder obtained by grinding in step S4 has a particle size of less than or equal to 2 μm.
Compared with the prior art, the invention has the beneficial effects that: vanadium, silicon, titanium and the like in the waste SCR catalyst are all recovered, the recovery rate is high, vanadium, silicon, titanium and the like are recovered by acid dissolution of oxalic acid, hydrofluoric acid and sulfuric acid with different strengths, vanadium pentoxide is easily dissolved in oxalic acid, silicon dioxide and hydrofluoric acid to form gas silicon fluoride, the arsenic oxide and the hydrofluoric acid form arsenic fluoride insoluble substances, the arsenic fluoride insoluble substances are removed in ethanol cleaning, titanium dioxide and sulfuric acid react to form titanium sulfate, and a surfactant is added to adjust the pore structure of titanium tungsten powder. The recovery rate of vanadium is more than 99 percent, the recovery rate of titanium and tungsten is more than 95 percent, the recovery rate of silicon dioxide is less than 0.5 percent, and the specific surface area of the recovered titanium-tungsten powder is 90m2More than g, pore volume greater than 0.3cm3The impurity Fe, K, Na and As is less than 100ug/g, and the three-step acid leaching process avoids the defects of single acid leaching element mixing, and low leaching rate and recovery rate due to mutual interference among elements.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Method for recovering titanium-tungsten powder from waste SCR catalystThe method comprises the following steps: (1) grinding, physically sieving and sorting the waste SCR catalyst to obtain waste catalyst powder with the granularity less than 5 mu m; (2) acid leaching in one step: adding oxalic acid with the concentration of 20% into the waste SCR catalyst, leaching at the temperature of 95 ℃, reacting for 2.0h, adding the oxalic acid with the vanadium molar ratio of 1:2, filtering to obtain a vanadium oxalate solution at the end point of leaching when the total amount of vanadium in filter residue is less than 0.01%, evaporating, crystallizing and filtering to obtain a vanadium oxalate product, wherein the recovery rate of vanadium reaches 99.3%. (3) Acid leaching in the second step: adding 0.5mol/L hydrofluoric acid into the filter residue in the last step for acid leaching, wherein the leaching temperature is 80 ℃, reacting for 1.5h, the adding amount of the hydrofluoric acid is 1.05 times of the theoretical required amount of silicon, the content of silicon dioxide in the filter residue is detected to be 0.45% by an X-ray fluorescence analyzer (XRF) at the leaching end point, recovering gaseous silicon fluoride, adding ethanol, cleaning and removing arsenic, and detecting by an inductively coupled plasma emission spectrometer (ICP) until the content of the arsenic is 87 ug/g. (4) Acid leaching in three steps: adding 50% sulfuric acid solution into the filter residue in the last step for acid leaching, wherein the leaching temperature is 120 ℃, reacting for 5.0h, the adding amount of sulfuric acid is 1.1 times of the theoretical required amount of titanium, the reaction end point takes the total amount of titanium in the filter residue to be less than 0.1%, filtering to obtain titanium sulfate solution, adding 0.1% P123, precipitating with ammonia water, removing Fe, K and Na together with the filter residue through an ionic membrane, calcining for 6h at 400 ℃, and grinding titanium tungsten powder product with the particle size of 1.35 mu m. The recovery rates of titanium and tungsten were 96.7% and 95.2%. The content of Fe, K and Na in the titanium tungsten powder product is respectively 90ug/g, 78ug/g and 98ug/g through ICP detection. Beckmann specific surface area and aperture analyzer detection specific surface area 95.32m2G, pore volume 0.35cm3/g。
Example 2
A method for recovering titanium tungsten powder from a waste SCR catalyst comprises the following steps: (1) grinding, physically sieving and sorting the waste SCR catalyst to obtain waste catalyst powder with the granularity less than 5 mu m; (2) acid leaching in one step: adding oxalic acid with the concentration of 30% into the waste SCR catalyst, leaching at the temperature of 85 ℃, reacting for 3.0h, adding the oxalic acid with the vanadium molar ratio of 1:5, filtering to obtain a vanadium oxalate solution at the end point of leaching when the total vanadium content in the filter residue is less than 0.01%, evaporating, crystallizing and filtering to obtain a vanadium oxalate product, wherein the recovery rate of vanadium reaches 99.5%. (3) Acid leaching in the second step: adding the filter residue in the last step0.5mol/L hydrofluoric acid is subjected to acid leaching at the leaching temperature of 90 ℃, the reaction is carried out for 1.0h, the addition amount of the hydrofluoric acid is 1.1 times of the theoretical required amount of silicon, the content of silicon dioxide in filter residue is detected to be 0.35% by an X-ray fluorescence analyzer (XRF) at the leaching end point, gaseous silicon fluoride is recovered, ethanol is added, arsenic is removed by cleaning, and an inductively coupled plasma emission spectrometer (ICP) is used for detecting until the content of the arsenic is 67 ug/g. (4) Acid leaching in three steps: adding a 60% sulfuric acid solution into the filter residue in the last step for acid leaching, wherein the leaching temperature is 180 ℃, reacting for 3.5 hours, the adding amount of sulfuric acid is 1.2 times of the theoretical required amount of titanium, the reaction end point takes the total amount of titanium in the filter residue to be less than 0.1%, filtering to obtain a titanium sulfate solution, adding 0.05% hexadecyl trimethyl ammonium hydroxide, precipitating with ammonia water, removing Fe, K and Na with the filter residue through an ionic membrane, calcining for 4 hours at 550 ℃, and grinding the titanium-tungsten powder product to have the particle size of 1.41 mu m. The recovery rates of titanium and tungsten were 97.1% and 96.3%, respectively. The content of Fe, K and Na in the titanium tungsten powder product is respectively 87ug/g, 78ug/g and 88ug/g through ICP detection. Beckmann specific surface area and aperture analyzer detection specific surface area 102.01m2G, pore volume 0.41cm3/g。
Example 3
A method for recovering titanium tungsten powder from a waste SCR catalyst comprises the following steps: (1) grinding, physically sieving and sorting the waste SCR catalyst to obtain waste catalyst powder with the granularity less than 5 mu m; (2) acid leaching in one step: adding oxalic acid with the concentration of 25% into the waste SCR catalyst, leaching at the temperature of 90 ℃, reacting for 3.0h, adding the oxalic acid with the vanadium molar ratio of 1:4, filtering to obtain a vanadium oxalate solution at the end point of leaching when the total amount of vanadium in filter residue is less than 0.01%, evaporating, crystallizing and filtering to obtain a vanadium oxalate product, wherein the recovery rate of vanadium reaches 99.6%. (3) Acid leaching in the second step: adding 0.8mol/L hydrofluoric acid into the filter residue in the last step for acid leaching, wherein the leaching temperature is 90 ℃, reacting for 1.5h, the adding amount of the hydrofluoric acid is 1.05 times of the theoretical required amount of silicon, detecting the content of silicon dioxide in the filter residue to be 0.28% by an X-ray fluorescence analyzer (XRF) at the leaching end point, recovering gaseous silicon fluoride, adding ethanol, cleaning and removing arsenic, and detecting by an inductively coupled plasma emission spectrometer (ICP) until the content of the arsenic is 56 ug/g. (4) Acid leaching in three steps: adding 55% sulfuric acid solution into the filter residue in the last step, and acid leaching at 160 deg.CAnd reacting for 4.0h, adding sulfuric acid in an amount which is 1.15 times of the theoretical required amount of titanium, filtering to obtain a titanium sulfate solution at the end point of the reaction, wherein the total amount of titanium in the filter residue is less than 0.1%, adding 0.06% of dodecyl dimethyl primary amine, precipitating with ammonia water, removing Fe, K and Na together with the filter residue through an ionic membrane, calcining for 5h at 500 ℃, and grinding the titanium-tungsten powder product to obtain the titanium-tungsten powder with the particle size of 1.68 mu m. The recovery rates of titanium and tungsten were 96.7% and 95.2%. The content of Fe, K and Na in the titanium tungsten powder product is respectively 78ug/g, 87ug/g and 95ug/g through ICP detection. Beckmann specific surface area and aperture analyzer detection specific surface area 99.21m2G, pore volume 0.38cm3/g。
Example 4
A method for recovering titanium tungsten powder from a waste SCR catalyst comprises the following steps: (1) grinding, physically sieving and sorting the waste SCR catalyst to obtain waste catalyst powder with the granularity less than 5 mu m; (2) acid leaching in one step: adding oxalic acid with the concentration of 30% into the waste SCR catalyst, leaching at the temperature of 90 ℃, reacting for 2.0h, adding the oxalic acid with the vanadium molar ratio of 1:3, filtering to obtain a vanadium oxalate solution at the end point of leaching when the total vanadium content in the filter residue is less than 0.01%, evaporating, crystallizing and filtering to obtain a vanadium oxalate product, wherein the recovery rate of vanadium reaches 99.5%. (3) Acid leaching in the second step: adding 0.9mol/L hydrofluoric acid into the filter residue in the last step for acid leaching, wherein the leaching temperature is 90 ℃, reacting for 1.0h, the adding amount of the hydrofluoric acid is 1.05 times of the theoretical required amount of silicon, the content of silicon dioxide in the filter residue is detected to be 0.39% by an X-ray fluorescence analyzer (XRF) at the leaching end point, recovering gaseous silicon fluoride, adding ethanol, cleaning and removing arsenic, and detecting by an inductively coupled plasma emission spectrometer (ICP) until the content of the arsenic is 95 ug/g. (4) Acid leaching in three steps: adding a 60% sulfuric acid solution into the filter residue in the last step for acid leaching, wherein the leaching temperature is 140 ℃, reacting for 5.0h, the adding amount of sulfuric acid is 1.1 times of the theoretical required amount of titanium, the reaction end point takes the total amount of titanium in the filter residue to be less than 0.1%, filtering to obtain a titanium sulfate solution, adding 0.08% tetradecyl dimethyl primary amine, precipitating with ammonia water, removing Fe, K and Na with the filter residue through an ionic membrane, calcining for 5h at 500 ℃, and grinding the titanium-tungsten powder product to have the particle size of 1.35 mu m. The recovery rates of titanium and tungsten were 96.7% and 95.2%. The ICP detection shows that Fe, K and Na of the titanium tungsten powder product are respectively 97ug/g, 86ug/g and 96ug/g. Specific surface area detected by Beckmann and specific surface area detected by aperture analyzer 93.35m2G, pore volume 0.37cm3/g。
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. A method for recovering titanium tungsten powder from a waste SCR catalyst is characterized by comprising the following steps: the method comprises the following steps:
s1: grinding the waste SCR catalyst and then screening to obtain waste catalyst powder with the granularity less than 5 mu m;
s2: adding oxalic acid with the concentration of 20% -30% into the waste catalyst powder obtained in the step S1 for acid leaching, filtering to obtain a vanadium oxalate solution, evaporating, crystallizing and filtering to obtain a vanadium oxalate product, wherein the leaching temperature is 85-95 ℃, and the leaching end point is that the total content of vanadium in filter residue is less than 0.01%;
s3: adding 0.5-1 mol/L hydrofluoric acid into the filter residue in the S2 for acid leaching, wherein the leaching temperature is 80-90 ℃, the adding amount of the hydrofluoric acid is 1.05-1.1 times of the theoretical required amount of silicon, the reaction time is 1.0-1.5h, the end point of the leaching is that the total amount of the metal silicon in the filter residue is less than 0.5 percent, recovering the gaseous silicon fluoride, adding ethanol, and cleaning to remove arsenic until the content of the arsenic is less than 100 ug/g;
s4: and adding 50-60% sulfuric acid solution into the filter residue in the S3 for acid leaching, wherein the leaching temperature is 120-180 ℃, the reaction end point is that the total titanium content in the filter residue is less than 0.1%, filtering to obtain titanium sulfate solution, adding a surfactant, precipitating with ammonia water, removing impurities together with the filter residue to remove Fe, K and Na, calcining at high temperature, and grinding to obtain titanium-tungsten powder.
2. The method of claim 1, wherein the method comprises the following steps: the oxalic acid is added in the step S2 in a vanadium molar ratio of 1:2-1:5, and the reaction time is 2.0-3.0 h.
3. The method of claim 1, wherein the method comprises the following steps: the adding amount of the sulfuric acid in the step S4 is 1.1-1.2 times of the theoretical required amount of the titanium, and the reaction time is 3.5-5.0 h.
4. The method of claim 1, wherein the method comprises the following steps: in the step S4, the surfactant is any one of (polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer) P123, cetyl trimethyl ammonium hydroxide, and primary amine, and the addition amount of the surfactant is 0.1% to 0.3% of the solution amount.
5. The method of claim 1, wherein the method comprises the following steps: the temperature of the high-temperature calcination in the step S4 is 400-550 ℃, and the calcination time is 4-6 h.
6. The method of claim 1, wherein the method comprises the following steps: and in the step S4, the titanium-tungsten powder is ground to obtain the titanium-tungsten powder with the particle size less than or equal to 2 microns.
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| CN110923459B (en) | 2021-02-05 |
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