CN103031438B - Recovery process for rare earth and noble metal in automobile tail gas purification catalyst - Google Patents
Recovery process for rare earth and noble metal in automobile tail gas purification catalyst Download PDFInfo
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- CN103031438B CN103031438B CN201110297722.4A CN201110297722A CN103031438B CN 103031438 B CN103031438 B CN 103031438B CN 201110297722 A CN201110297722 A CN 201110297722A CN 103031438 B CN103031438 B CN 103031438B
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention relates to the waste and old resource reuse, in particular to a recovery process for rare earth and noble metal in automobile tail gas purification catalyst. The method comprises the following steps of: (1) grinding; (2) roasting; (3) washing with hot water; (4) carrying out acid dissolving; (5) recovering cobalt and nickel, and extracting to separate rare earth, such as cerium, praseodymium, lanthanum and yttrium; (6) recovering platinum; and (7) recovering palladium and rhodium. Compared with the prior art, the recovery process has the characteristics that the rare earth in the waste and old rare earth automobile tail gas purification catalyst is recovered, the noble metal is recovered, and the recovery process has the advantages of high rare earth and noble earth recovery rate, low equipment requirement and low production cost, and the method is simple and easy to realize.
Description
Technical field
The present invention relates to waste and old resource reutilization, be specifically related to the recovery process of a kind of cleaning catalyst for tail gases of automobiles middle-weight rare earths and precious metal.
Background technology
Rare earth cleaning catalyst for tail gases of automobiles because price is low, higher, the long service life of Heat stability is good, activity, in purifying vehicle exhaust field, enjoy favor, rare earth cleaning catalyst for tail gases of automobiles is more and more widely used.The type of the rare-earth type cleaning catalyst for tail gases of automobiles of widespread use at present mainly contains two kinds: perovskite typed and cerium zirconium sosoloid.
Cleaning catalyst for tail gases of automobiles be take and made cellular pottery or metal is matrix, and honeycomb internal surface is coated with by Al
2o
3, rare earth based material (CeO
2mixed oxide with other metal oxide) and the activated coating that forms of three constituent elements of a small amount of precious metal (platinum, palladium or rhodium).
Be 5～8 years the working life of general rare-earth type cleaning catalyst for tail gases of automobiles, comprise that China is often close on the rare-earth type cleaning catalyst for tail gases of automobiles of 1,000,000 abandoned car the inside, in these catalyzer, contain rare-earth element cerium, praseodymium, lanthanum, yttrium etc. and precious metal palladium, platinum, rhodium, also have aluminium, molybdenum, vanadium, cobalt, nickel, iron, strontium, zirconium etc.Metal ion major part exists with oxide compound or metal oxygen acid group form.
Existingly to reclaiming the method for metal in waste and old rare earth cleaning catalyst for tail gases of automobiles, mainly contain wet method, pressure cyanide method and plasmamelt process.But existing Wet technique is lower to the precious metal rate of recovery, and difficult low-grade material, precious metal reclaimed not thorough.And pressure cyanide method is utilized directly selectivity leaching recovery platinum metals from spent auto-catalysts of prussiate high-temperature pressurizing, but prussiate belongs to violent in toxicity, control strictly, and difficult management, facility investment is large.And plasmamelt process exists metal and slag separation difficulty, equipment requirements high, plasma gun is short work-ing life, the problem that cost is high.And the rare earth element of above-mentioned each method in all can not efficient recovery cleaning catalyst for tail gases of automobiles.
Summary of the invention
The present invention, for solving above-mentioned shortcoming of the prior art, provides the recovery process of a kind of cleaning catalyst for tail gases of automobiles middle-weight rare earths and precious metal, and the method comprises the following steps:
(1) waste and old rare earth cleaning catalyst for tail gases of automobiles is ground to whole mistake 80～150 mesh sieves;
(2) waste and old rare earth cleaning catalyst for tail gases of automobiles powder is mixed to roasting between 300 ℃～500 ℃, roasting time 2～4 hours according to mass ratio 1: 0.8～1.5 with sodium hydroxide;
(3) with material after the hot wash roasting of 60～99 ℃, solid-to-liquid ratio 1: 3～6, agitator treating 2～4 hours;
(4) filter, from filtrate, reclaim aluminium, molybdenum, vanadium, zirconium etc., filter residue dissolves with acid, in order to dissolve the metallic elements such as rare earth element and cobalt ferronickel, hydrogen ion concentration is 0.5～2mol/l, 60～99 ℃ of temperature of reaction, 2～4 hours reaction times, solid-to-liquid ratio 1: 3～6; And then filtration obtains the solution that contains rare earth and iron-cobalt-nickel ion and the filter residue that contains precious metal;
(5) solution that contains rare earth and iron-cobalt-nickel ion that step (4) obtains after filtering, between first regulator solution pH value to 3.5～4.5, then under 20～40 ℃ of conditions, add sulfide or pass into hydrogen sulfide, the mole number of sulphur is 1.0～1.2 times of cobalt ferronickel total mole number, react 2～4 hours, cobalt ferronickel is precipitated completely; The cobalt ferronickel throw out that precipitation obtains further reclaims cobalt nickel again; The sedimentary filtrate of elimination cobalt nickel is the solution that contains rare earth, with rare earths such as P507 extracting and separating cerium, praseodymium, lanthanum, yttriums, then prepares rare earth oxide;
(6) with the mixing solutions of hydrochloric acid and clorox, leach the precious metal slag of step (4), obtain the solution that contains palladium, platinum, rhodium, in the situation that guaranteeing that clorox is excessive, adding sodium hydroxide or potassium hydroxide to return adjust pH is 4～8, make palladium, rhodium form hydrous oxide precipitation, the pure platinum solution then obtaining again refining obtains metal platinum;
(7) precipitation that contains palladium rhodium obtaining, with after dissolving with hydrochloric acid, is used N530 extraction of palladium, and with the hydrochloric acid back extraction of 5～7mol/l, the palladium solution obtaining again electrorefining obtains palladium metal; In raffinate, contain rhodium, then with hydrazine hydrate reduction, obtain metal rhodium.
Wherein,
Step (1) is ground waste and old rare earth cleaning catalyst for tail gases of automobiles, is preferably and all crosses 100～120 mesh sieves.
Step (2) is preferably waste and old rare earth cleaning catalyst for tail gases of automobiles powder according to mass ratio 1: 1～1.2 and mixes with sodium hydroxide.
When step (4) is dissolved the metallic elements such as rare earth element and cobalt ferronickel with acid, better hydrogen ion concentration is 1～1.5mol/l.
When step (4) is dissolved the metallic elements such as rare earth element and cobalt ferronickel with acid, solid-to-liquid ratio is preferably 1: 4～and 5.
Compared with prior art, the present invention had both reclaimed waste and old rare earth cleaning catalyst for tail gases of automobiles middle-weight rare earths, also reclaimed precious metal, and high to rare earth and the precious metal rate of recovery, and method is simple, equipment requirements is low, and production cost is low, economic benefit is large, has realized the comprehensive reutilization of resource.The present invention leaches initial gross separation the enrichment of real precious metal, rare earth metal and other metals by substep, with hydrochloric acid and hypochlorous leaching precious metal, avoided chloroazotic acid leaching, has reduced the loss of equipment, has reduced cost simultaneously.
Accompanying drawing explanation
Fig. 1 is technical process reference drawing of the present invention.
Embodiment
Some embodiments of the present invention are below provided, to help further, understand the present invention, but protection scope of the present invention are not limited in these embodiment.
Embodiment 1
Fig. 1 is technical process reference drawing of the present invention, and technical process concrete steps are as shown in the figure as follows:
(1) spent catalyst is ground to whole mistake 80～150 mesh sieves.
(2) spent catalyst powder is mixed to roasting between 300 ℃～500 ℃, roasting time 2～4 hours according to mass ratio 1: 0.8～1.5 with sodium hydroxide.
(3) with material after the hot wash roasting of 60～99 ℃, solid-to-liquid ratio 1: 3～6, agitator treating 2～4 hours.
(4) filter, filtrate is reclaimed aluminium, molybdenum, vanadium, zirconium etc.In filter residue, contain rare earth, precious metal, cobalt ferronickel etc.Filter residue dissolves with acid, and in order to dissolve the metallic elements such as rare earth element and cobalt ferronickel, hydrogen ion concentration is 0.5～2mol/l, 60～99 ℃ of temperature of reaction, 2～4 hours reaction times, solid-to-liquid ratio 1: 3～1: 6.In filter residue, be mainly the precious metals such as palladium platinum rhodium.
(5) the first regulator solution pH of the solution value that step (4) contains rare earth and iron-cobalt-nickel ion is between 3.5～4.5, then at 20～40 ℃, add sulfide or pass into hydrogen sulfide, react 2～4 hours, cobalt ferronickel is precipitated completely, and the mole number of sulphur is 1.0～1.2 times of cobalt ferronickel mole number.The cobalt ferronickel throw out that precipitation obtains further reclaims cobalt nickel again.The solution that filtrate being contained rare earth, with rare earths such as P507 extracting and separating cerium, praseodymium, lanthanum, yttriums, then prepares rare earth oxide.
(6) with the mixing solutions of hydrochloric acid and clorox, leach the precious metal slag of step (4), obtain the solution that contains palladium, platinum, rhodium, in the situation that guaranteeing that clorox is excessive, add sodium hydroxide or potassium hydroxide to go back to adjust pH to 4～8, make palladium, rhodium form hydrous oxide precipitation, the pure platinum solution then obtaining again refining obtains metal platinum.
(7) precipitation that contains palladium rhodium obtaining, with after dissolving with hydrochloric acid, is used N530 extraction of palladium, and with the hydrochloric acid back extraction of 5～7mol/l, the palladium solution obtaining again electrorefining obtains palladium metal.In raffinate, contain rhodium, available hydrazine hydrate reduction obtains metal rhodium.
Embodiment 2
(1) spent catalyst is ground to whole mistake 100 mesh sieves.
(2) spent catalyst powder is mixed at 1: 1.0 to roasting between 400 ℃, roasting time 3 hours according to mass ratio with sodium hydroxide.
(3) with material after the hot wash roasting of 85 ℃, solid-to-liquid ratio 1: 4, agitator treating 3 hours.
(4) filter, filtrate is reclaimed aluminium, molybdenum, vanadium, zirconium etc.In filter residue, contain rare earth, precious metal, cobalt ferronickel etc.Filter residue sulfuric acid dissolution, in order to dissolve the metallic elements such as rare earth element and cobalt ferronickel, hydrogen ion concentration is 1.0mol/l, 85 ℃ of temperature of reaction, 3 hours reaction times, solid-to-liquid ratio 1: 4.In filter residue, be mainly the precious metals such as palladium platinum rhodium.
(5) the first regulator solution pH of the solution value that step (4) contains rare earth and iron-cobalt-nickel ion is 3.5, then at 30 ℃, adds sodium sulphite, reacts 3 hours, and cobalt ferronickel is precipitated completely, and the mole number of sulphur is 1.1 times of cobalt ferronickel mole number.The cobalt ferronickel throw out that precipitation obtains further reclaims cobalt nickel again.The solution that filtrate being contained rare earth, with rare earths such as P507 extracting and separating cerium, praseodymium, lanthanum, yttriums, then prepares rare earth oxide.
(6) with the mixing solutions of hydrochloric acid and clorox, leach the precious metal slag of step (4), hydrochloric acid with the mole number of clorox, the ratio of the mole number of palladium platinum rhodium 1: 1: 0.3, solid-to-liquid ratio 1: 2,70 ℃ of reactions 2 hours, obtain the solution that contains palladium, platinum, rhodium, in the situation that guaranteeing that clorox is excessive, adding sodium hydroxide or potassium hydroxide readjustment pH is 4, make palladium, rhodium form hydrous oxide precipitation, the pure platinum solution then obtaining again refining obtains metal platinum.
(7) precipitation that contains palladium rhodium obtaining, with after dissolving with hydrochloric acid, is used N530 extraction of palladium, through 3 grades of extractions, and organic/water 1: 0.5, with the salt of 7mol/l, 4 grades of back extractions, the palladium solution obtaining again electrorefining obtains palladium metal.In raffinate, contain rhodium, available hydrazine hydrate reduction obtains metal rhodium.
The total yield 97% of final rare earth, the rate of recovery of palladium, platinum, rhodium is respectively 96%, 94%, 93%.
Embodiment 3
(1) spent catalyst is ground to whole mistake 80 mesh sieves.
(2) spent catalyst powder is mixed at 1: 0.8 to roasting between 300 ℃, roasting time 2 hours according to mass ratio with sodium hydroxide.
(3) with material after the hot wash roasting of 60 ℃, solid-to-liquid ratio 1: 3, agitator treating 2 hours.
(4) filter, filtrate is reclaimed aluminium, molybdenum, vanadium, zirconium etc.In filter residue, contain rare earth, precious metal, cobalt ferronickel etc.Filter residue dissolves with acid, and in order to dissolve the metallic elements such as rare earth element and cobalt ferronickel, hydrogen ion concentration is 0.5mol/l, 60 ℃ of temperature of reaction, 2 hours reaction times, solid-to-liquid ratio 1: 3.In filter residue, be mainly the precious metals such as palladium platinum rhodium.
(5) the first regulator solution pH of solution that step (4) contains rare earth and iron-cobalt-nickel ion is 3.5, then at 20 ℃, add sulfide or pass into hydrogen sulfide, react 2 hours, cobalt ferronickel is precipitated completely, the mole number of sulphur is 1.0 times of cobalt ferronickel mole number.The cobalt ferronickel throw out that precipitation obtains further reclaims cobalt nickel again.The solution that filtrate being contained rare earth, with rare earths such as P507 extracting and separating cerium, praseodymium, lanthanum, yttriums, then prepares rare earth oxide.
(6) with the mixing solutions of hydrochloric acid and clorox, leach the precious metal slag of step (4), obtain the solution that contains palladium, platinum, rhodium, in the situation that guaranteeing that clorox is excessive, adding sodium hydroxide or potassium hydroxide readjustment pH is 4, make palladium, rhodium form hydrous oxide precipitation, the pure platinum solution then obtaining again refining obtains metal platinum.
(7) precipitation that contains palladium rhodium obtaining, with after dissolving with hydrochloric acid, is used N530 extraction of palladium, and with the hydrochloric acid back extraction of 5mol/l, the palladium solution obtaining again electrorefining obtains palladium metal.In raffinate, contain rhodium, available hydrazine hydrate reduction obtains metal rhodium.
The total yield 96% of final rare earth, the rate of recovery of palladium, platinum, rhodium is respectively 95%, 92%, 92%.
Embodiment 4
(1) spent catalyst is ground to whole mistake 150 mesh sieves.
(2) spent catalyst powder is mixed at 1: 1.5 to roasting between 500 ℃, roasting time 4 hours according to mass ratio with sodium hydroxide.
(3) with material after the hot wash roasting of 99 ℃, solid-to-liquid ratio 1: 6, agitator treating 4 hours.
(4) filter, filtrate is reclaimed aluminium, molybdenum, vanadium, zirconium etc.In filter residue, contain rare earth, precious metal, cobalt ferronickel etc.Filter residue dissolves with acid, and in order to dissolve the metallic elements such as rare earth element and cobalt ferronickel, hydrogen ion concentration is 2mol/l, 99 ℃ of temperature of reaction, 4 hours reaction times, solid-to-liquid ratio 1: 5.In filter residue, be mainly the precious metals such as palladium platinum rhodium.
(5) the first regulator solution pH of solution that step (4) contains rare earth and iron-cobalt-nickel ion is 4.5, then at 40 ℃, add sulfide or pass into hydrogen sulfide, react 4 hours, cobalt ferronickel is precipitated completely, the mole number of sulphur is 1.2 times of cobalt ferronickel mole number.The cobalt ferronickel throw out that precipitation obtains further reclaims cobalt nickel again.The solution that filtrate being contained rare earth, with rare earths such as P507 extracting and separating cerium, praseodymium, lanthanum, yttriums, then prepares rare earth oxide.
(6) with the mixing solutions of hydrochloric acid and clorox, leach the precious metal slag of step (4), obtain the solution that contains palladium, platinum, rhodium, in the situation that guaranteeing that clorox is excessive, adding sodium hydroxide or potassium hydroxide readjustment pH is 6, make palladium, rhodium form hydrous oxide precipitation, the pure platinum solution then obtaining again refining obtains metal platinum.
(7) precipitation that contains palladium rhodium obtaining, with after dissolving with hydrochloric acid, is used N530 extraction of palladium, and with the hydrochloric acid back extraction of 6mol/l, the palladium solution obtaining again electrorefining obtains palladium metal.In raffinate, contain rhodium, available hydrazine hydrate reduction obtains metal rhodium.
The total yield 98% of final rare earth, the rate of recovery of palladium, platinum, rhodium is respectively 96%, 95%, 93%.
Embodiment 5
(1) spent catalyst is ground to whole mistake 120 mesh sieves.
(2) spent catalyst powder is mixed at 1: 1.2 to roasting between 400 ℃, roasting time 3 hours according to mass ratio with sodium hydroxide.
(3) with material after the hot wash roasting of 85 ℃, solid-to-liquid ratio 1: 4, agitator treating 3 hours.
(4) filter, filtrate is reclaimed aluminium, molybdenum, vanadium, zirconium etc.In filter residue, contain rare earth, precious metal, cobalt ferronickel etc.Filter residue dissolves with acid, and in order to dissolve the metallic elements such as rare earth element and cobalt ferronickel, hydrogen ion concentration is 1.5mol/l, 85 ℃ of temperature of reaction, 3 hours reaction times, solid-to-liquid ratio 1: 4.In filter residue, be mainly the precious metals such as palladium platinum rhodium.
(5) the first regulator solution pH of solution that step (4) contains rare earth and iron-cobalt-nickel ion is 4, then at 35 ℃, add sulfide or pass into hydrogen sulfide, react 3 hours, cobalt ferronickel is precipitated completely, the mole number of sulphur is 1.1 times of cobalt ferronickel mole number.The cobalt ferronickel throw out that precipitation obtains further reclaims cobalt nickel again.The solution that filtrate being contained rare earth, with rare earths such as P507 extracting and separating cerium, praseodymium, lanthanum, yttriums, then prepares rare earth oxide.
(6) with the mixing solutions of hydrochloric acid and clorox, leach the precious metal slag of step (4), obtain the solution that contains palladium, platinum, rhodium, in the situation that guaranteeing that clorox is excessive, adding sodium hydroxide or potassium hydroxide readjustment pH is 5, make palladium, rhodium form hydrous oxide precipitation, the pure platinum solution then obtaining again refining obtains metal platinum.
(7) precipitation that contains palladium rhodium obtaining, with after dissolving with hydrochloric acid, is used N530 extraction of palladium, and with the hydrochloric acid back extraction of 6mol/l, the palladium solution obtaining again electrorefining obtains palladium metal.In raffinate, contain rhodium, available hydrazine hydrate reduction obtains metal rhodium.
The total yield 96% of final rare earth, the rate of recovery of palladium, platinum, rhodium is respectively 95%, 94%, 93%.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (5)
1. a recovery process for cleaning catalyst for tail gases of automobiles middle-weight rare earths and precious metal, is characterized in that, comprises the following steps:
(1) waste and old rare earth cleaning catalyst for tail gases of automobiles is ground to whole mistake 80～150 mesh sieves;
(2) waste and old rare earth cleaning catalyst for tail gases of automobiles powder is mixed to roasting between 300 ℃～500 ℃, roasting time 2～4 hours according to mass ratio 1:0.8～1.5 with sodium hydroxide;
(3) with material after the hot wash roasting of 60～99 ℃, solid-to-liquid ratio 1:3～6, agitator treating 2～4 hours;
(4) filter, from filtrate, reclaim aluminium, molybdenum, vanadium, zirconium, filter residue dissolves with acid, and in order to dissolve rare earth element and cobalt ferronickel metallic element, hydrogen ion concentration is 0.5～2mol/l, 60～99 ℃ of temperature of reaction, 2～4 hours reaction times, solid-to-liquid ratio 1:3～6; And then filtration obtains the solution that contains rare earth and iron-cobalt-nickel ion and the filter residue that contains precious metal;
(5) solution that contains rare earth and iron-cobalt-nickel ion that step (4) obtains after filtering, between first regulator solution pH value to 3.5～4.5, then under 20～40 ℃ of conditions, add sulfide or pass into hydrogen sulfide, the mole number of sulphur is 1.0～1.2 times of cobalt ferronickel total mole number, react 2～4 hours, cobalt ferronickel is precipitated completely; The cobalt ferronickel throw out that precipitation obtains further reclaims cobalt nickel again; The sedimentary filtrate of elimination cobalt nickel is the solution that contains rare earth, with P507 extracting and separating cerium, praseodymium, lanthanum, yttrium rare earth, then prepares rare earth oxide;
(6) with the mixing solutions of hydrochloric acid and clorox, leach the filter residue containing precious metal of step (4), obtain the solution that contains palladium, platinum, rhodium, in the situation that guaranteeing that clorox is excessive, adding sodium hydroxide or potassium hydroxide to return adjust pH is 4～8, make palladium, rhodium form hydrous oxide precipitation, the pure platinum solution then obtaining again refining obtains metal platinum;
(7) precipitation that contains palladium rhodium obtaining, with after dissolving with hydrochloric acid, is used N530 extraction of palladium, and with the hydrochloric acid back extraction of 5～7mol/l, the palladium solution obtaining again electrorefining obtains palladium metal; In raffinate, contain rhodium, then with hydrazine hydrate reduction, obtain metal rhodium.
2. the recovery process of cleaning catalyst for tail gases of automobiles middle-weight rare earths according to claim 1 and precious metal, is characterized in that, step (1) is ground waste and old rare earth cleaning catalyst for tail gases of automobiles, whole mistake 100～120 mesh sieves.
3. the recovery process of cleaning catalyst for tail gases of automobiles middle-weight rare earths according to claim 1 and precious metal, is characterized in that, step (2) is mixed with sodium hydroxide waste and old rare earth cleaning catalyst for tail gases of automobiles powder according to mass ratio 1:1～1.2.
4. the recovery process of cleaning catalyst for tail gases of automobiles middle-weight rare earths according to claim 1 and precious metal, is characterized in that, when step (4) is dissolved rare earth element and cobalt ferronickel metallic element with acid, hydrogen ion concentration is 1～1.5mol/l.
5. the recovery process of cleaning catalyst for tail gases of automobiles middle-weight rare earths according to claim 1 and precious metal, is characterized in that, when step (4) is dissolved rare earth element and cobalt ferronickel metallic element with acid, and solid-to-liquid ratio 1:4～5.
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| CN105567972A (en) * | 2014-10-10 | 2016-05-11 | 清华大学 | Method for recovering rare earth elements from spent catalyst |
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| CN112899478A (en) * | 2021-01-13 | 2021-06-04 | 深圳市正力实业有限公司 | Device and method for efficiently purifying precious metals in waste automobile exhaust catalyst |
| CN113215590A (en) * | 2021-04-25 | 2021-08-06 | 郴州百一环保高新材料有限公司 | Platinum element extraction process for waste ternary catalyst based on electrolytic reaction |
| CN114381610B (en) * | 2022-01-27 | 2023-07-21 | 湖南省南铂新材料有限公司 | Environment-friendly efficient recovery method for noble metal of waste automobile catalyst |
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Effective date of registration: 20151231 Address after: 301600, No. ten, No. 9, Jinghai circular economy industrial zone, Ziya County, Tianjin Patentee after: Green U.S. (Tianjin) city mineral products circulation industry development company limited Address before: 518000, room 20, building 2008, building A, Wing Tai Binhai building, Xinghua Road, South Central, Xinghua Road, Baoan District, Shenzhen, Guangdong, Baoan Patentee before: Shenzhen GEM High-tech Co., Ltd. Patentee before: Jingmen GEM New Material Co., Ltd. |