CN110055423A - A method of platinum group metal and rare earth in enrichment failure cleaning catalyst for tail gases of automobiles - Google Patents
A method of platinum group metal and rare earth in enrichment failure cleaning catalyst for tail gases of automobiles Download PDFInfo
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- CN110055423A CN110055423A CN201910437568.2A CN201910437568A CN110055423A CN 110055423 A CN110055423 A CN 110055423A CN 201910437568 A CN201910437568 A CN 201910437568A CN 110055423 A CN110055423 A CN 110055423A
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- rare earth
- automobiles
- acidleach
- tail gases
- cleaning catalyst
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Classifications
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
-
- 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
- C22B59/00—Obtaining rare earth metals
-
- 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
-
- 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
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
-
- 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
A method of platinum group metal and rare earth in enrichment failure cleaning catalyst for tail gases of automobiles, the present invention will carry out pressure leaching after failure cleaning catalyst for tail gases of automobiles fine grinding in sodium hydroxide solution, and make γ-A1 therein2O3It is partly dissolved and converts the readily soluble sodalite of acid system for the cordierite carrier in catalyst；The pressure leaching slag of output carries out acidic leaching, and rare earth element enters in acid leaching solution, and platinum, palladium, rhodium element is retained in slag, realizes the separation of platinum, palladium, rhodium and rare earth；Sodium sulphate is added in oxytropism leachate and forms the compound salt precipitating of sulfuric acid rare earth, recovering rare earth element, and acid insoluble slag is then further processed recycling platinum, palladium, rhodium metal.The leaching rate of lanthanum and yttrium of the present invention reaches 95% or more, and the platinum, palladium, rhodium in the cleaning catalyst for tail gases of automobiles that fails is enriched with 13 times or more, is conducive to the subsequent extracted of noble metal, lanthanum and yttrium comprehensive recovery reach 90% or more.
Description
Technical field
The present invention relates to hydrometallurgy process in field of metallurgy, are a kind of effectively enrichment failure cleaning catalyst for tail gases of automobiles
The method of middle platinum group metal and rare earth.
Background technique
Automobile catalyst is the important channel for controlling motor vehicle exhaust emission in fuel oil motor supply shop industry, reducing pollution.It is main at present
The automobile catalyst of stream is by carrier (2MgO2A12O3·5SiO2Or 2FeO2A12O3·0.5SiO2), surface covering (γ-
A12O3), active material (Pt, Pd and Rh) and auxiliary agent (rare earths such as Ce, La, Ba, Sr, Zr or alkaline earth element oxide) composition,
Wherein the content of noble metal is generally 0.05% or more, and contains about 4% ~ 8% rare earth element.Present platinum family annual in the world
Metal production is in 300t or so, wherein 90% derives from national, the platinum group metal reserves in China and the yield poles such as Russia and South Africa
It is few, less than the 1% of worldwide production.Platinum group metal effectively in recycling secondary resource is the effective way for solving the problems, such as shortage of resources
One of diameter, therefore study and recycle platinum group metal and rare earth from the automobile catalyst of failure with very positive meaning.
According to the chemical composition and nature difference of catalyst, many researchers are in order to recycle in cleaning catalyst for tail gases of automobiles
Valuable metal propose different processing methods.There are addition flux and oxidant to mix with automobile catalyst, after high-temperature calcination
The mode of leaching recycles valuable metal；Also have and recycle valuable metal by way of sulfating roasting；For the vapour of metallic carrier
Vehicle catalyst has using the method for high melt and carries out recycling valuable metal.
In patent of invention CN102899498A(Zhang Zebiao, one kind is waited to leach platinum from failure cleaning catalyst for tail gases of automobiles
The method China of race's metal, 201210368339.8 [P] .2013-01-30) in, after spent catalyst is crushed fine grinding, it is added
Flux (NaHSO4) and oxidant (NaClO or NaClO3), high-temperature calcination after mixing, then the water logging of calcined product room temperature, takes
Oxidant (H is added in filter residue2O2) and hydrochloric acid carry out acidleach, filtration washing obtains the solution containing platinum group metal platinum, palladium, rhodium.The invention
All very high to the leaching rate of platinum group metal, the leaching rate of especially rhodium element has reached 99% or more, but impurity element in solution
Content is high, and later separation and extraction are more difficult, is unable to get effective application.
In patent of invention CN105671304A(Dong Haigang, one kind is waited to recycle from failure cleaning catalyst for tail gases of automobiles dilute
The method China of soil and platinum group metal, 201610102182.2 [P] .2016-06-15) in, failure purifying vehicle exhaust is urged
After agent fine grinding, is mixed with sulfuric acid and carry out sulfating roasting, then carry out acidleach with dilute sulfuric acid, the recovering rare earth member from pickle liquor
Element recycles platinum group metal from acid leaching residue.The invention carries out recycling valuable metal, operating environment by the way of sulfidation roasting
Difference, to the seriously polluted of environment.
In patent of invention CN106282568A(Fan Xingxiang, wait one kind rich from spent automotive exhaust catalysts metallic carrier
Collect the method China of platinum group metal, 201510285196.8 [P] .2017-01-04) in, using high temperature melting failure car tail
Gas cleaning catalyst, then cooling again or atomization is dusted, and forms tiny alloy, then acid adding Selectively leaching alkali metal, is passed through
Filtering and washing, obtain platinum group metal concentrate, realize the efficiently concentrating of platinum group metal.The invention does not need additionally to add any
Trapping agent, and it is easy to operate, but need using high temperature melting furnaces such as plasma electric stoves, the demand to energy consumption is larger, meanwhile,
This method has certain limitation, and the catalyst for handling cordierite carrier, which needs to add additional trapping agent, could extract it
In valuable metal.
Summary of the invention
The purpose of the present invention is to provide platinum, palladium, rhodium and rare earths in a kind of efficiently concentrating failure cleaning catalyst for tail gases of automobiles
The method of element.
The present invention in order to achieve the above object the technical solution adopted is that: will failure cleaning catalyst for tail gases of automobiles fine grinding after
Pressure leaching is carried out in sodium hydroxide solution, makes γ-A1 therein2O3It is partly dissolved and carries the cordierite in catalyst
Body is converted into the readily soluble sodalite of acid system；The pressure leaching slag of output carries out acidic leaching, and rare earth element enters acidity
In leachate, and platinum, palladium, rhodium element is still retained in slag, realizes the separation of platinum, palladium, rhodium and rare earth；It is added in oxytropism leachate
Sodium sulphate forms the compound salt precipitating of sulfuric acid rare earth, thus recovering rare earth element, acid insoluble slag is then further processed recycling platinum palladium
The metals such as rhodium.
Specific technical process and technical parameter are as follows:
1. alkaline pressure of oxygen leaching
Failure cleaning catalyst for tail gases of automobiles is broken and to be finely ground to particle size range be 0.149mm or less, then will be levigate after mistake
Effect catalyst is added in autoclave after mixing with sodium hydroxide solution, and quality control is added as failure car tail in sodium hydroxide
0.5 ~ 3.0 times of gas cleaning catalyst quality, liquid-solid ratio (liquid volume mL and failure cleaning catalyst for tail gases of automobiles quality g it
Than) it is 3 ~ 8:1, mixing speed is 300 ~ 600rpm, is heated to 150 ~ 250 DEG C, reacts 2 ~ 4h；After completion of the reaction, it is filtered, washed
Afterwards, pressureleaching solution and pressure leaching slag are obtained.
2. acidleach
By the 1.0 ~ 4.0mol/L hydrochloric acid solution acidleach of pressure leaching slag, liquid-solid ratio (liquid volume mL and pressure leaching slag are controlled
The ratio between quality g) be 5 ~ 15:1, then be added reducing agent hydrazine hydrate, hydrazine hydrate volume fraction control be liquor capacity 0.1% ~
0.5%, leaching time is 0.5 ~ 4.0h, and acidleach temperature is 50 ~ 90 DEG C, and mixing speed is 300 ~ 600rpm；After completion of the reaction, mistake
Acidleach leachate and acidleach insoluble slag are obtained after filter, washing；Acidleach leachate be used for recovering rare earth element, acidleach insoluble slag then into
One step recycles platinum group.
3. double salt precipitation
It is added between sodium hydrate regulator solution pH to 0.5 ~ 3.0 into acidleach leachate, sodium sulphate is added later, control sulfuric acid
Sodium quality is 3 ~ 10:1 of rare earth quality in solution, and reaction temperature is 50 ~ 70 DEG C, and the reaction time is 15 ~ 60min, mixing speed
For 300 ~ 600rpm.Filtration washing drying, obtains sulfuric acid rare earth double salt precipitation.
The sodium hydroxide, sodium sulphate, hydrochloric acid, hydrazine hydrate are technical grade reagent.
In the failure cleaning catalyst for tail gases of automobiles, mass content: Al 5.0% ~ 30.0%, Si 5.0% ~ 30.0%,
La 0.1% ~ 5.0%, Y 0.01% ~ 2.0%, Ce 1.0% ~ 15.0%, 20.0 ~ 500.0g/t of Pt, 30.0 ~ 800.0g/t of Pd, Rh
5.0~300.0g/t。
The present invention has the advantage that (1) relative to traditional failure cleaning catalyst for tail gases of automobiles recovery and treatment method
Pressure leaching can make the cordierite carrier of indissoluble in catalyst be converted into the readily soluble sodalite of acid system, pressure leaching slag salt
When acid solution leaches, for the leaching rate of aluminium and silicon greater than 94%, the leaching rate of lanthanum and yttrium reaches 95% or more, keeps failure vehicle exhaust net
The platinum, palladium, rhodium changed in catalyst is enriched with 13 times or more, is conducive to the subsequent extracted of noble metal；(2) heavy by acidic leaching and double salt
It forms sediment and the recycling of rare earth element can be achieved, wherein lanthanum and yttrium comprehensive recovery reach 90% or more；(3) alkaline pressure leaching pair
The corrosion of equipment is small, safe operation, and valuable metal synthetical recovery is profitable；(4) labor intensity of the invention is low, handles the time
Short, good operational environment.
Detailed description of the invention
Fig. 1: process flow chart of the invention.
Specific embodiment
Embodiment 1
The specific ingredient of catalyst: Al 17.97%, Si 17.78%, La 0.58%, Y 0.28%, Ce 4.02%, Pt 113.5g/t,
Pd 212g/t、Rh 73g/t。
Industrial sodium hydroxide, NaOH content >=96%；Technical grade sulfuric acid sodium, Na2SO4Content >=96%；Technical grade salt
Acid, HCl content are 36% ~ 38%；Technical grade hydrazine hydrate, N2H4·H2O content is >=80%.
Granularity after fine grinding is taken to be less than the failure cleaning catalyst for tail gases of automobiles 15.00g of 0.149mm, with 12.00g hydroxide
It is added in autoclave after sodium mixing, the deionized water of 75mL is then added, control mixing speed is 400rpm, slow heating
To 150 DEG C, 3.0h is reacted；After completion of the reaction, filtration washing obtains pressureleaching solution 200mL and pressure leaching slag 19.03g.Add
Press ammonium acetate are as follows: Si 2.38g/L, Al 2.47g/L, La 9.50mg/L, Y 2.50mg/L, Ce 10.00mg/L, platinum palladium
Rhodium content is substantially zeroed.Wherein pressure leaching slag slag rate is 126.87%, and the leaching rate of cerium, lanthanum and yttrium is respectively 0.33%, 2.18%
With 1.19%.
Above-mentioned pressure leaching slag 10.00g is taken, with 150mL 1.5mol/L hydrochloric acid solution acidleach, hydrazine hydrate 0.15mL is added,
Leaching time is 2h, and acidleach temperature is 80 DEG C, mixing speed 400rpm；After completion of the reaction, it is filtered, washed to obtain acidleach leaching
Liquid 250mL and acidleach insoluble slag 1.01g.Acidleach ammonium acetate are as follows: Al 4.38g/L, Si 4.37g/L, La 170.48mg/
L, Y 83.63mg/L, Ce 404.87mg/L.Acidleach insoluble slag slag rate is 10.10%, and the leaching rate of aluminium and silicon is respectively 94.85%
With 94.63%, the leaching rate of lanthanum and yttrium is respectively 95.30% and 95.87%；Platinum, palladium, rhodium are enriched in substantially in acidleach insoluble slag, point
It is not enriched 13.74 times, 13.61 times and 13.58 times.Acidleach insoluble slag further extracts platinum group metal.
200mL acidleach leachate is taken, it is 2.0 that appropriate sodium hydroxide to pH value of solution is added thereto, adds sodium sulphate
0.70g, reaction temperature are 50 DEG C, mixing speed 300rpm, reaction time 15min.After completion of the reaction, filtration washing is filtered
Liquid 300mL and precipitating 0.41g.Filtrate component are as follows: La 3.40mg/L, Y 1.40mg/L, Ce 6.93mg/L, cerium, lanthanum and yttrium
Rate of deposition is respectively 97.66%, 97.01% and 97.49%.Lanthanum and yttrium comprehensive recovery are respectively 92.48% and 93.42%.
Embodiment 2
The specific ingredient of catalyst: Si 17.82%, Al 17.94%, La 0.60%, Y 0.29%, Ce 4.12%, Pt 115.4g/t,
Pd 221.5g/t、Rh 78.2g/t。
Industrial sodium hydroxide, NaOH content >=96%；Technical grade sulfuric acid sodium, Na2SO4Content >=96%；Technical grade salt
Acid, HCl content are 36% ~ 38%；Technical grade hydrazine hydrate, N2H4·H2O content is >=80%.
Granularity after fine grinding is taken to be less than the failure cleaning catalyst for tail gases of automobiles 15.00g of 0.149mm, with 30.00g hydroxide
It is added in autoclave after sodium mixing, the deionized water of 90mL is then added, control mixing speed is 600rpm, slow heating
To 200 DEG C, 4.0h is reacted；After completion of the reaction, filtration washing obtains pressureleaching solution 200mL and pressure leaching slag 19.06g.Add
Press ammonium acetate are as follows: Al 2.45g/L, Si 2.41g/L, La 9.98mg/L, Y 3.01mg/L, Ce 14.98mg/L, platinum palladium
Rhodium content is substantially zeroed.Wherein pressure leaching slag slag rate is 127.07%, and the leaching rate of cerium, lanthanum and yttrium is respectively 0.49%, 2.22%
With 1.38%.
Above-mentioned pressure leaching slag 10.00g is taken, with 100mL 3.0mol/L hydrochloric acid solution acidleach, hydrazine hydrate 0.50mL is added,
Leaching time is 1.5h, and acidleach temperature is 60 DEG C, mixing speed 600rpm；After completion of the reaction, it is filtered, washed to obtain acidleach leaching
Liquid 250mL and acidleach insoluble slag 1.03g out.Acidleach ammonium acetate are as follows: Al 4.37g/L, Si 4.36g/L, La
175.48mg/L, Y 85.63mg/L, Ce 448.26mg/L.Acidleach insoluble slag slag rate is 10.30%, and the leaching rate of aluminium and silicon is
94.67% and 94.84%, the leaching rate of lanthanum and yttrium is 95.02% and 95.11%；Platinum, palladium, rhodium are enriched in substantially in acidleach insoluble slag,
Its enrichment times is respectively 13.52 times, 13.48 times and 13.94 times.Acidleach insoluble slag further extracts platinum group metal.
200mL acidleach leachate is taken, it is 2.2 that appropriate sodium hydroxide to pH value of solution is added thereto, adds sodium sulphate
1.00g, reaction temperature are 60 DEG C, mixing speed 500rpm, reaction time 20min.After completion of the reaction, it is filtered, washed and is filtered
Liquid 300mL and precipitating 0.43g.Filtrate component are as follows: La 3.41mg/L, Y 1.50mg/L, Ce 8.62mg/L, cerium, lanthanum and yttrium
Rate of deposition is 97.12%, 97.09% and 97.37%.Lanthanum and yttrium comprehensive recovery are 92.29% and 92.58%.
Claims (3)
1. a kind of method of platinum group metal and rare earth in enrichment failure cleaning catalyst for tail gases of automobiles, it is characterised in that including following
Step:
A. alkaline pressure of oxygen leaching
Failure cleaning catalyst for tail gases of automobiles is crushed and is finely ground to 0.149mm or less, then will be levigate after spent catalyst
It is added in autoclave after being mixed with sodium hydroxide solution, sodium hydroxide is added quality control and urges for failure purifying vehicle exhaust
0.5 ~ 3.0 times of agent quality, liquid-solid ratio, i.e. liquid volume mL and failure the ratio between cleaning catalyst for tail gases of automobiles quality g for 3 ~
8:1, mixing speed are 300 ~ 600rpm, are heated to 150 ~ 250 DEG C, react 2 ~ 4h；After completion of the reaction, it after being filtered, washed, obtains
Pressureleaching solution and pressure leaching slag；
B. acidleach
By the 1.0 ~ 4.0mol/L hydrochloric acid solution acidleach of pressure leaching slag, liquid-solid ratio, i.e. liquid volume mL and pressure leaching are controlled
The ratio between slag amount g is 5 ~ 15:1, and reducing agent hydrazine hydrate is then added, and hydrazine hydrate volume fraction is the 0.1% ~ 0.5% of liquor capacity,
Leaching time is 0.5 ~ 4.0h, and acidleach temperature is 50 ~ 90 DEG C, and mixing speed is 300 ~ 600rpm；After completion of the reaction, it filters, wash
Acidleach leachate and acidleach insoluble slag are obtained after washing；Acidleach leachate is used for recovering rare earth element, and acidleach insoluble slag is then further
Recycle platinum group；
C. double salt precipitation
Sodium hydrate regulator solution pH to 0.5 ~ 3.0 is added into acidleach leachate, adds sodium sulphate, controls sodium sulfate quality
For 3 ~ 10:1 of rare earth quality in solution, reaction temperature is 50 ~ 70 DEG C, and the reaction time is 15 ~ 60min, mixing speed is 300 ~
600rpm, filtration washing drying, obtains sulfuric acid rare earth double salt precipitation.
2. the method for platinum group metal and rare earth, special in enrichment failure cleaning catalyst for tail gases of automobiles as described in claim 1
Sign is: sodium hydroxide, sodium sulphate, hydrochloric acid and the hydrazine hydrate is technical grade reagent.
3. the method for platinum group metal and rare earth, special in enrichment failure cleaning catalyst for tail gases of automobiles as described in claim 1
Sign is: in the failure cleaning catalyst for tail gases of automobiles, element mass percentage are as follows: Al 5.0% ~ 30.0%, Si
5.0% ~ 30.0%, La 0.1% ~ 5.0%, Y 0.01% ~ 2.0%, Ce 1.0% ~ 15.0%, 20.0 ~ 500.0g/t of Pt, Pd 30.0 ~
5.0 ~ 300.0g/t of 800.0g/t and Rh.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111334676A (en) * | 2020-03-24 | 2020-06-26 | 河北天蓝环保科技有限公司 | Treatment method of spent rare earth-containing catalyst |
| CN112501439A (en) * | 2020-10-22 | 2021-03-16 | 贵研资源（易门）有限公司 | Pretreatment method of iron alloy containing precious metal |
| CN112921181A (en) * | 2021-01-26 | 2021-06-08 | 广东省科学院资源综合利用研究所 | Method for recovering platinum group metal in automobile waste catalyst |
| CN113088704A (en) * | 2021-04-07 | 2021-07-09 | 江苏北矿金属循环利用科技有限公司 | Method for recovering precious metal from glass fiber refractory brick |
| CN113234931A (en) * | 2021-05-14 | 2021-08-10 | 昆明理工大学 | Failure Pt/Al2O3Method for comprehensively recovering platinum and aluminum from catalyst |
| CN113293301A (en) * | 2021-05-21 | 2021-08-24 | 北京科技大学 | Method for recovering platinum group metals from metal carrier waste automobile exhaust catalyst |
| CN114934180A (en) * | 2022-04-12 | 2022-08-23 | 中南大学 | Method for enriching ruthenium in alumina-based waste ruthenium-loaded catalyst |
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| CN105671304A (en) * | 2016-02-25 | 2016-06-15 | 昆明贵金属研究所 | Method for recycling rare earth and platinum group metal from spent automobile emission purification catalyst |
| CN107287438A (en) * | 2017-06-06 | 2017-10-24 | 中南大学 | Cordierite type waste automobile exhaust three-way catalyst crude extraction method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111334676A (en) * | 2020-03-24 | 2020-06-26 | 河北天蓝环保科技有限公司 | Treatment method of spent rare earth-containing catalyst |
| CN112501439A (en) * | 2020-10-22 | 2021-03-16 | 贵研资源（易门）有限公司 | Pretreatment method of iron alloy containing precious metal |
| CN112921181A (en) * | 2021-01-26 | 2021-06-08 | 广东省科学院资源综合利用研究所 | Method for recovering platinum group metal in automobile waste catalyst |
| CN113088704A (en) * | 2021-04-07 | 2021-07-09 | 江苏北矿金属循环利用科技有限公司 | Method for recovering precious metal from glass fiber refractory brick |
| CN113088704B (en) * | 2021-04-07 | 2022-05-24 | 江苏北矿金属循环利用科技有限公司 | Method for recovering precious metal from glass fiber refractory brick |
| CN113234931A (en) * | 2021-05-14 | 2021-08-10 | 昆明理工大学 | Failure Pt/Al2O3Method for comprehensively recovering platinum and aluminum from catalyst |
| CN113293301A (en) * | 2021-05-21 | 2021-08-24 | 北京科技大学 | Method for recovering platinum group metals from metal carrier waste automobile exhaust catalyst |
| CN114934180A (en) * | 2022-04-12 | 2022-08-23 | 中南大学 | Method for enriching ruthenium in alumina-based waste ruthenium-loaded catalyst |
| CN114934180B (en) * | 2022-04-12 | 2023-01-24 | 中南大学 | Method for enriching ruthenium in alumina-based waste ruthenium-loaded catalyst |
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|---|---|
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