CN114058853B - Method for recovering titanium, vanadium and tungsten from waste SCR denitration catalyst - Google Patents
Method for recovering titanium, vanadium and tungsten from waste SCR denitration catalyst Download PDFInfo
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- CN114058853B CN114058853B CN202111422901.6A CN202111422901A CN114058853B CN 114058853 B CN114058853 B CN 114058853B CN 202111422901 A CN202111422901 A CN 202111422901A CN 114058853 B CN114058853 B CN 114058853B
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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
- C22B7/006—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
- C22B34/10—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
- C22B34/125—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 containing a sulfur ion as active agent
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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
- C22B34/10—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
- C22B34/1259—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 treatment or purification of titanium containing solutions or liquors or slurries
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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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
- C22B34/225—Obtaining vanadium from spent catalysts
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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
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
- C22B34/365—Obtaining tungsten from spent catalysts
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention provides a method for recovering titanium, vanadium and tungsten from waste denitration catalysts, which comprises the following steps: dedusting and crushing the waste denitration catalyst, carrying out acidolysis on waste catalyst powder by using concentrated sulfuric acid, leaching an acidolysis product, adding titanium, tungsten and vanadium in the waste catalyst into a leaching solution, extracting the titanium and the tungsten in the leaching solution by using a weakly alkaline extractant, carrying an organic phase, carrying titanium by using sulfuric acid and hydrogen peroxide, and carrying tungsten by using ammonia water after titanium stripping; after the vanadium-containing raffinate is returned to leach acidolysis products to improve the vanadium concentration, part of vanadium is extracted and recovered in an open circuit. The invention provides a method for synchronously leaching valuable elements of titanium, vanadium and tungsten in a waste catalyst by using sulfuric acid as a leaching agent; tungsten and titanium in the leachate are co-extracted by using a weakly alkaline extractant, hydrogen peroxide and sulfuric acid are used as a titanium-resisting agent, and ammonia water is used as a tungsten-resisting agent, so that the separation of titanium, tungsten and vanadium in the decomposition liquid is realized. The method has simple process and high technical and economic indexes.
Description
Technical Field
The invention relates to the field of resource circulation and the field of nonferrous metallurgy, in particular to a method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst.
Background
Selective Catalytic Reduction (SCR) is widely used for flue gas denitration by domestic thermal power plants because of its excellent performance. The catalyst can be deactivated to form a waste catalyst in a complex environment for about 3 years because of various factors, and the waste catalyst is classified as a dangerous waste because the waste catalyst contains about 1 percent of vanadium pentoxide and trace arsenic trioxide. The composite material contains about 85% of titanium dioxide, about 1% of vanadium pentoxide and 3-5% of tungsten trioxide, and if the composite material can be comprehensively recovered, the composite material not only can solve the environmental problem caused by stacking or landfill and reduce resource consumption, but also can produce economic benefits. At present, the recovery of the waste catalyst is widely carried out by adopting an alkali roasting or alkali pressure leaching method, and the problems of high energy consumption, high alkali consumption, low leaching rate of tungsten and vanadium, independent recovery of titanium dioxide and the like exist. The method for efficiently and comprehensively recovering valuable elements in the waste catalyst has high economic and environmental values.
The waste SCR catalyst can be prepared into products such as titanium dioxide (titanium dioxide), ammonium paratungstate, vanadium pentoxide and the like through comprehensive recovery, and the titanium dioxide has great application value in the fields of metallurgy, chemical industry and the like, and is widely applied to the aspects of manufacturing coatings, high-grade white paint, white rubber, synthetic fibers, welding electrodes, denitration catalysts and the like. Vanadium is an important strategic metal, and is widely used as a grain refiner and a deoxidizer in the field of producing high-quality alloys, such as various iron alloys and titanium alloys, due to the properties of grain refinement and oxygen affinity. Tungsten is also an important strategic metal and is widely used for manufacturing high-melting-point alloys, hard alloys and the like.
Disclosure of Invention
The invention aims to provide a method for efficiently leaching valuable elements in a waste catalyst at one time by using low-cost sulfuric acid as a leaching agent and separating the valuable elements in a leaching solution to produce a corresponding product, and solves the problems that the existing alkaline leaching method is high in cost, low in tungsten and vanadium leaching rate and required to separately leach and recover titanium dioxide.
The invention provides a method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst, which sequentially comprises the following steps: (1) Blowing the waste denitration catalyst by using compressed air and washing the waste denitration catalyst by using tap water to remove dust in a pore channel of the waste denitration catalyst, and then crushing and grinding the waste denitration catalyst to obtain waste catalyst powder with a certain granularity; (2) Taking catalyst powder with a certain mass in an acidolysis pot, and then mixing the waste catalyst and concentrated sulfuric acid according to the mass ratio of 1:1.4 to 2.0, adding dilute sulphuric acid into the mixture to dilute the mixture to 70 to 95 percent to release heat, heating the mixture to carry out acidolysis, keeping the temperature at 180 to 250 ℃ and reacting for 1.5 to 2.5 hours; leaching the obtained acidolysis product by using vanadium-containing raffinate or waste acid obtained in the step (3), wherein the leaching temperature is 25-75 ℃, the leaching time is 40-70 min, and the leaching rates of titanium, vanadium and tungsten are all higher than 96%; (3) Extracting titanium and tungsten from the leachate containing titanium, vanadium and tungsten by using a weakly alkaline extractant such as N1923, and leaving vanadium in a raffinate; (4) The titanium and tungsten loaded organic phase is eluted by using 0.5 to 2mol/L mixed solution of sulfuric acid and hydrogen peroxide, the molar ratio of hydrogen peroxide to titanium is 1.5 to 3, tungsten still remains in the organic phase, and the obtained titanium-containing eluent is used for extracting titanium; (5) Reversely extracting tungsten from the tungsten-containing organic phase after titanium elution by using 2-4 mol/L ammonia water to obtain an ammonium tungstate solution for extracting tungsten; (6) After pH value of the vanadium-containing raffinate is adjusted by cyclic enrichment, vanadium is extracted by using cation extracting agents such as P204 and the like, and the vanadium is recovered after acid or alkali back extraction.
Compared with the prior art, the method takes sulfuric acid as an acidolysis and leaching agent to perform acidolysis leaching on the waste SCR denitration catalyst, so that titanium, vanadium and tungsten can be efficiently leached at the same time, the leaching rate can reach more than 96%, the leachate is extracted and back-extracted by using a weakly alkaline extractant, the titanium and tungsten can be separated, vanadium in raffinate is circularly enriched and pH is adjusted, and then P204 and the like are used for extraction and back-extraction, so that the recovery of vanadium can be realized. The pure oxides of titanium, vanadium and tungsten can be prepared by the subsequent operations of precipitation, crystallization and the like.
Detailed Description
The method for recovering titanium, vanadium and tungsten from waste denitration catalysts sequentially comprises two parts of acidolysis and leaching, titanium and tungsten extraction separation and vanadium extraction recovery, and for the purpose of describing the content of the invention in detail, specific implementation modes of each part of the invention are respectively illustrated as follows:
1. acidolysis and leaching of waste catalyst
Example one
The invention provides a method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst, which comprises the following steps of:
(1) Blowing the waste denitration catalyst by using compressed air and washing the waste denitration catalyst by using tap water to remove dust in a pore channel of the waste denitration catalyst, and then crushing and grinding the waste denitration catalyst to obtain waste catalyst powder with the particle size of 140 meshes.
(2) Taking catalyst powder with a certain mass in an acidolysis pot, and adding the catalyst powder into the acidolysis pot according to the weight ratio of the waste catalyst: the mass ratio of concentrated sulfuric acid is 1:1.4 adding concentrated sulfuric acid, adding water to dilute the sulfuric acid to 95 percent, heating the mixture for acidolysis, wherein the reaction temperature is 250 ℃, and the reaction time is 2.5 hours.
(3) Adding vanadium-containing raffinate into titanyl sulfate solid obtained after acidolysis to leach, wherein the solid-to-liquid ratio of leaching liquid is 5, the leaching temperature is 25 ℃, the leaching time is 70min, and the leaching rates of titanium, vanadium and tungsten can reach more than 96.5%.
Example two
The invention provides a method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst, which sequentially comprises the following steps:
(1) Blowing the waste denitration catalyst by using compressed air and washing the waste denitration catalyst by using tap water to remove dust in a pore channel, and then crushing and grinding the waste denitration catalyst to obtain waste catalyst powder with the granularity of 120 meshes.
(2) Taking a certain mass of catalyst powder in an acidolysis pot, and adding the catalyst powder into the acidolysis pot according to the weight ratio of the waste catalyst: the mass ratio of concentrated sulfuric acid is 1:1.8 adding concentrated sulfuric acid, adding water to dilute the sulfuric acid to 85 percent, heating for acidolysis, wherein the reaction temperature is 200 ℃, and the reaction time is 2 hours.
(3) Adding vanadium-containing raffinate into titanyl sulfate solid obtained after acidolysis to leach, wherein the solid-to-solid ratio of a leaching solution is 4, the leaching temperature is 45 ℃, the leaching time is 60min, and the leaching rates of titanium, vanadium and tungsten can reach more than 97%.
EXAMPLE III
The invention provides a method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst, which sequentially comprises the following steps of:
(1) Blowing the waste denitration catalyst by using compressed air and washing the waste denitration catalyst by using tap water to remove dust in a pore channel, and then crushing and grinding the waste denitration catalyst to obtain waste catalyst powder with the granularity of 100 meshes.
(2) Taking a certain mass of catalyst powder in an acidolysis pot, and adding the catalyst powder into the acidolysis pot according to the weight ratio of the waste catalyst: the mass ratio of concentrated sulfuric acid is 1:2 adding concentrated sulfuric acid, adding water to dilute the sulfuric acid to 70 percent, heating and carrying out acidolysis, wherein the reaction temperature is 180 ℃, and the reaction time is 1.5h.
(3) Adding vanadium-containing raffinate into titanyl sulfate solid obtained after acidolysis to leach, wherein the solid-to-solid ratio of a leaching solution is 6, the leaching temperature is 75 ℃, the leaching time is 40min, and the leaching rates of titanium, vanadium and tungsten can reach more than 97.5%.
2. Extracting and separating titanium, vanadium and tungsten from leachate
Example one
The invention provides a method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst, which comprises the following steps of:
(1) Extracting titanium and tungsten from titanium, vanadium and tungsten-containing feed liquid obtained by acidolysis leaching by using N1923, wherein the volume concentration of N1923 is 20%, the concentration of sec-octanol is 2%, and the balance is sulfonated kerosene, under the condition that the O/A =3 is compared, through 5-stage countercurrent extraction, the extraction rates of titanium and tungsten reach more than 99.6% and 99%, and the extraction rate of vanadium is less than 3%.
(2) And (2) performing back extraction by using 0.5mol/L sulfuric acid and hydrogen peroxide, wherein the molar weight ratio of the hydrogen peroxide to the titanium is 1.5, performing 5-stage counter-current back extraction when the O/A =2, wherein the back extraction rate of the titanium is higher than 97%, the back extraction rate of the tungsten is less than 5%, and the back extraction solution is concentrated and crystallized to prepare the metatitanic acid.
(3) And washing the tungsten-containing organic phase subjected to titanium removal with tap water to carry sulfuric acid, performing back extraction of tungsten by using 2mol/L ammonia water, and crystallizing the back extraction solution to obtain ammonium paratungstate.
(4) The raffinate after enriching vanadium was adjusted to pH 2 by adding calcium hydroxide paste, extracted vanadium using 10% P204+5% TBP, and the vanadium extraction rate reached 98.5% or more by grade 5 counter current extraction.
(5) And (3) carrying out back extraction on the vanadium-containing load organic phase by using 1mol/L sulfuric acid, adding ammonia into the back extraction solution to adjust the pH value to 2, precipitating vanadium to obtain ammonium polyvanadate, and calcining to obtain vanadium pentoxide.
Example two
The invention provides a method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst, which comprises the following steps of:
(1) Titanium and tungsten in the titanium, vanadium and tungsten-containing feed liquid obtained by acidolysis leaching are extracted by N1923, wherein the volume concentration of N1923 is 40%, the concentration of secondary octanol is 2%, and the balance is sulfonated kerosene, and under the condition that the O/A =3, the extraction rate of titanium and tungsten is up to 99% and more than 99.2%, and the extraction rate of vanadium is less than 2.5% through 3-stage countercurrent extraction.
(2) 2mol/L sulfuric acid and hydrogen peroxide are used for back extraction, the molar weight ratio of the hydrogen peroxide to the titanium is 2.5, 6-stage counter-current back extraction is carried out at O/A =2, the titanium back extraction rate is higher than 98%, the tungsten back extraction rate is less than 4%, and the back extraction solution is concentrated and crystallized to prepare metatitanic acid.
(3) And washing the tungsten-containing organic phase subjected to titanium removal with tap water to carry sulfuric acid, performing back extraction of tungsten by using 4mol/L ammonia water, and crystallizing the back extraction solution to obtain ammonium paratungstate.
(4) The raffinate after enriching vanadium is added with calcium hydroxide paste to adjust pH to 2, vanadium is extracted by using 10% P204+5% TBP, and the vanadium extraction rate reaches more than 99% through 6-grade countercurrent extraction.
(5) And (3) carrying out back extraction on the vanadium-containing load organic phase by using 1.5mol/L sulfuric acid, adding ammonia into the back extraction solution to adjust the pH value to 2, precipitating vanadium to obtain ammonium polyvanadate, and calcining to obtain vanadium pentoxide.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (3)
1. A method for recovering titanium, vanadium and tungsten from a waste SCR denitration catalyst is characterized by comprising the following steps:
(1) Blowing and washing the waste denitration catalyst to remove impurity dust, and crushing and grinding the waste denitration catalyst to obtain waste catalyst powder;
(2) Mixing and decomposing waste catalyst powder, concentrated sulfuric acid and water according to a certain proportion, leaching the acidolyzed material by using waste acid, water or vanadium-containing raffinate to obtain leachate containing titanium, vanadium and tungsten; in the step (2), the ratio of the waste catalyst powder to the concentrated sulfuric acid is 1.4-2.0, the mixed material is diluted by adding water until the concentration of the sulfuric acid is 70-95%, and the mixed material is heated to start decomposition, the decomposition temperature is 180-250 ℃, and the decomposition time is more than 1.5 hours; in the step (2), leaching the decomposed material by using vanadium-containing raffinate or waste acid generated in the step (3), wherein the leaching temperature is 25-75 ℃, and the leaching time is 40-70 min;
(3) Extracting titanium and tungsten in the leachate containing titanium, vanadium and tungsten by using a weakly alkaline extractant, and leaving vanadium in the raffinate;
(4) Eluting titanium in the organic phase loaded with titanium and tungsten by using a mixed solution of sulfuric acid and hydrogen peroxide, wherein the tungsten still remains in the organic phase, and the obtained titanium-containing eluent is used for extracting titanium, wherein the concentration of sulfuric acid in the step (4) is 0.5-2 mol/L, and the molar weight ratio of the hydrogen peroxide to the titanium is 1.5-3;
(5) Reversely extracting tungsten from the tungsten-containing organic phase after titanium elution by using ammonia water to obtain an ammonium tungstate solution for extracting tungsten, wherein the concentration of the ammonia water in the step (5) is 2-4 mol/L;
(6) And (3) returning part of the vanadium-containing raffinate to the step (2) for recycling the enriched vanadium, and recovering part of the vanadium by adopting an extraction method.
2. The method for recovering titanium, vanadium and tungsten from the waste SCR denitration catalyst according to claim 1, which is characterized by comprising the following steps: and (3) simultaneously extracting titanium and tungsten from the leachate by using an organic phase, wherein the organic phase consists of a weakly alkaline extractant, a modifier and sulfonated kerosene, the weakly alkaline extractant comprises one or two of N1923 and N235, and the modifier comprises one or more of sec-octanol, isooctanol or TBP.
3. The method for recovering titanium, vanadium and tungsten from the waste SCR denitration catalyst according to claim 1, which is characterized by comprising the following steps: and (4) after pH of the vanadium-containing raffinate circularly enriched in the step (6) is adjusted, extracting vanadium by using a cationic extractant, and recovering vanadium from the vanadium by acid or alkali back extraction.
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| CN114921650A (en) * | 2022-03-29 | 2022-08-19 | 江门市崖门新财富环保工业有限公司 | Method for extracting metal from waste hydrogenation catalyst |
| CN115216649B (en) * | 2022-07-25 | 2023-06-09 | 中国石油大学(北京) | Method for preparing vanadium dioxide battery material by using waste vanadium-titanium-based SCR catalyst |
| CN115818718A (en) * | 2022-10-21 | 2023-03-21 | 中国科学院过程工程研究所 | Method for recycling titanium tungsten powder based on waste vanadium-titanium-tungsten SCR denitration catalyst |
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| CN104805298B (en) * | 2015-05-22 | 2018-01-16 | 中科过程（北京）科技有限公司 | A kind of recovery and treatment method of useless SCR denitration |
| CN104862485B (en) * | 2015-05-22 | 2017-08-18 | 中科过程（北京）科技有限公司 | A kind of vanadium of useless vanadium tungsten system SCR catalyst, tungsten separation and method of purification |
| CN107416902A (en) * | 2016-05-24 | 2017-12-01 | 北京清树科技发展有限公司 | A kind of method that low cost reclaims waste and old SCR denitration component materials |
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| CN111468103B (en) * | 2019-01-23 | 2021-07-20 | 中国科学院过程工程研究所 | Method for recycling waste SCR denitration catalyst to prepare new SCR denitration catalyst |
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