CN109722541A - A method of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles - Google Patents
A method of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles Download PDFInfo
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- CN109722541A CN109722541A CN201910169618.3A CN201910169618A CN109722541A CN 109722541 A CN109722541 A CN 109722541A CN 201910169618 A CN201910169618 A CN 201910169618A CN 109722541 A CN109722541 A CN 109722541A
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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
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Abstract
The invention discloses a kind of methods of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles, include the following steps, the curing of catalyst, separation, recovering rare earth, the roasting of platinum group metal and recycling platinum group metal, not only method is simple and easy by the present invention, improve rare earth and the platinum group metal rate of recovery, realize the comprehensive reutilization of rare precious metal secondary resource, the Al2O3 dissolution rate contained in catalyst can be made to be higher than 98%, the grade of platinum group metal concentrate is obtained 20% or so, its solubility property is fine, Oxidation Leaching is carried out in chloridric medium, the leaching rate of platinum group metal is up to 99.0%, chloride slag can return again to calcination process, the cost recovery of recovering rare earth and platinum group metal is saved.
Description
Technical field
The present invention relates to technical field, specially a kind of recovering rare earth and platinum family from failure cleaning catalyst for tail gases of automobiles
The method of metal.
Background technique
Cleaning catalyst for tail gases of automobiles is the most effective means for controlling motor vehicle exhaust emission, reducing pollution, the vapour containing rare earth
Tail gas cleaning catalyst price is low, thermal stability is good, it is active it is higher, there is preferable anti-poisoning capability, long service life, mesh
It is preceding to be used widely.Using cellular cordierite ceramic as matrix, honeycomb ceramics inner surface applies cleaning catalyst for tail gases of automobiles
It covers the γ-Al2O3 aluminum oxide coating layer of bigger serface, then load with rare earth sill (CeO2, La2O3 and other metal oxygens
The mixed oxide of compound) and a small amount of platinum group metal (platinum, palladium, rhodium) constitute active coating.
The recovery method of existing failure cleaning catalyst for tail gases of automobiles is mainly to recycle based on platinum group metal, including wet process
Technique (normal pressure dissolution method, pressure cyanide method etc.) and thermal process (lead method of trapping, copper trapping method, sulfonium method of trapping, plasma melting
Iron method of trapping, chloridising etc.).But the wet processing platinum group metal rate of recovery is low, scale application is also at home in thermal process
It is immature, there is investment greatly, equal series of problems at high cost.Importantly, above-mentioned each method cannot effectively recycle vehicle exhaust
Rare earth element in cleaning catalyst.
Summary of the invention
The purpose of the present invention is to provide one kind from failure cleaning catalyst for tail gases of automobiles in recovering rare earth and platinum group metal
Method to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme: it is a kind of from failure cleaning catalyst for tail gases of automobiles
The method of recovering rare earth and platinum group metal, includes the following steps,
(1) curing of catalyst: being to put at 1: 0.92 by the cleaning catalyst for tail gases of automobiles of failure and the concentrated sulfuric acid in mass ratio
Enter in reaction kettle and stir, and remain that the temperature of reaction kettle is 150 DEG C in whipping process, curing material is taken out after 5h；
(2) it separates: curing material obtained in step (1) being added water and stirred and leaches rare earth element, is warming up to 90 DEG C, constant temperature is anti-
6h is answered, reaction is completed to be diluted to solid-liquid mass ratio to be 1: 12, and cools the temperature to 60 DEG C and continue to stir, after reaction at ultrasound
Simultaneously sieving separating is managed, earth solution, the insoluble sediment in platinum group metal and catalyst carrier are respectively obtained；
(3) recovering rare earth: adding sodium sulphate to earth solution obtained in step (2), obtain sodium sulfate double salt sediment,
Double salt of rare earth is obtained by filtration later, prepares lanthanum, cerium mixed rare-earth oxide；
(4) roasting of platinum group metal: will be added sodium hydroxide solution in platinum group metal sediment obtained in step (2),
30-40min, repeated calcination 2-3 times are leached in 700-800 DEG C of roasting 7-8h of temperature, then with 10 times of boiling boiling；
(5) it recycles platinum group metal: the product that step (4) obtains being passed through chlorine and carries out potassium cloride, separation and purification work
After skill processing, platinum group metal platinum, palladium, rhodium are obtained.
Further, the catalyst in the step (1) passes through preheating before curing, and heating temperature is 1000-
1200 DEG C, heating time 3-4h.
Further, the mass ratio of curing material and water described in the step (2) is 1: 4.
Further, step (4) repeated calcination is 3 times.
Further, the concentration of the sodium hydroxide solution in the step (4) is 200-300g/L.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention leached by the curing of catalyst and separation, by earth solution and platinum group metal and other components
Initial gross separation, then sodium sulfate double salt sediment is obtained to earth solution filtered over sodium sulfate, then pass through roasting-dissolution method, Xiang Bo
Sodium hydroxide and chlorine are added in the insoluble sediment of race's metal, leaches platinum group metal, dissolved efficiency is high.
(2) present invention has both recycled the rare earth element in failure cleaning catalyst for tail gases of automobiles, has also recycled platinum therein
Race's metal, and rare earth and the platinum group metal rate of recovery are high, method is simple and easy, and production cost is low, high financial profit, realizes dilute expensive
The comprehensive reutilization of metal secondary resource.
(3) sodium hydroxide solution is added into platinum group metal sediment in heretofore described step (4), at 700 DEG C of temperature
7h is roasted, then leaches 30min with 10 times of boiling boiling, repeated calcination can make the Al2O3 dissolution rate contained in catalyst high three times
In 98%, the grade of platinum group metal concentrate is obtained 20% or so, solubility property is fine, and oxidation leaching is carried out in chloridric medium
Out, for the leaching rate of platinum group metal up to 99.0%, chloride slag can return again to calcination process, repeatable to recycle chlorine, save
The cost recovery of recovering rare earth and platinum group metal.
Therefore, not only method is simple and easy by the present invention, realizes the same of the comprehensive reutilization of rare precious metal secondary resource
When, rare earth and the platinum group metal rate of recovery are also improved, the Al2O3 dissolution rate contained in catalyst can be made to be higher than 98%, obtains platinum
For the grade of race's metal concentrate 20% or so, solubility property is fine, and Oxidation Leaching is carried out in chloridric medium, platinum group metal
For leaching rate up to 99.0%, chloride slag can return again to calcination process, save the cost recovery of rare earth and platinum group metal.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A method of from failure cleaning catalyst for tail gases of automobiles in recovering rare earth and platinum group metal, include the following steps,
(1) curing of catalyst: being to put at 1: 0.92 by the cleaning catalyst for tail gases of automobiles of failure and the concentrated sulfuric acid in mass ratio
Enter in reaction kettle and stir, and remain that the temperature of reaction kettle is 150 DEG C in whipping process, curing material is taken out after 5h；
(2) it separates: curing material obtained in step (1) being added water and stirred and leaches rare earth element, is warming up to 90 DEG C, constant temperature is anti-
6h is answered, reaction is completed to be diluted to solid-liquid mass ratio to be 1: 12, and cools the temperature to 60 DEG C and continue to stir, after reaction at ultrasound
Simultaneously sieving separating is managed, earth solution, the insoluble sediment in platinum group metal and catalyst carrier are respectively obtained；
(3) recovering rare earth: adding sodium sulphate to earth solution obtained in step (2), obtain sodium sulfate double salt sediment,
Double salt of rare earth is obtained by filtration later, prepares lanthanum, cerium mixed rare-earth oxide；
(4) roasting of platinum group metal: will be added sodium hydroxide solution in platinum group metal sediment obtained in step (2),
30min is leached in 700 DEG C of roasting 7h of temperature, then with 10 times of boiling boiling, repeated calcination 3 times；
(5) it recycles platinum group metal: the product that step (4) obtains being passed through chlorine and carries out potassium cloride, separation and purification work
After skill processing, platinum group metal platinum, palladium, rhodium are obtained.
In the present embodiment, the mass ratio of curing material and water described in the step (2) is 1: 4；
In the present embodiment, the catalyst in the step (1) passes through preheating before curing, and heating temperature is 1100
DEG C, heating time 3h；
In the present embodiment, step (4) repeated calcination is 3 times；
In the present embodiment, the concentration of the sodium hydroxide solution in the step (4) is 300g/L；
In the present embodiment, the overall recovery for measuring rare earth is 96.0%, platinum, palladium, rhodium the rate of recovery be respectively 98.0%,
99.0%, 96.0%.
Embodiment 2
2 difference from Example 1 of embodiment is:
The roasting of platinum group metal in the step (4): hydrogen-oxygen will be added in platinum group metal sediment obtained in step (2)
Change sodium solution, leaches 34min in 740 DEG C of roasting 7.7h of temperature, then with 10 times of boiling boiling；
Remaining is same as Example 1.
In the present embodiment, the overall recovery for measuring rare earth is 96.6%, platinum, palladium, rhodium the rate of recovery be respectively 97.5%,
99.1%, 95.7%.
Embodiment 3
3 difference from Example 1 of embodiment is:
The roasting of platinum group metal in the step (4): hydrogen-oxygen will be added in platinum group metal sediment obtained in step (2)
Change sodium solution, leaches 40min in 800 DEG C of roasting 8h of temperature, then with 10 times of boiling boiling；
Remaining is same as Example 1.
In the present embodiment, the overall recovery for measuring rare earth is 95.8%, platinum, palladium, rhodium the rate of recovery be respectively 97.7%,
98.6%, 96.6%.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art,
It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc.
With replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this
Within the protection scope of invention.
Claims (5)
1. a kind of method of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles, it is characterised in that: including
Following steps,
(1) curing of catalyst: by the cleaning catalyst for tail gases of automobiles of failure and the concentrated sulfuric acid be in mass ratio 1: 0.92 be put into it is anti-
It answers in kettle and stirs, and remain that the temperature of reaction kettle is 150 DEG C in whipping process, curing material is taken out after 5h；
(2) it separates: curing material obtained in step (1) being added water and stirred and leaches rare earth element, is warming up to 90 DEG C, isothermal reaction
6h, reaction is completed to be diluted to solid-liquid mass ratio to be 1: 12, and cools the temperature to 60 DEG C and continue to stir, and is ultrasonically treated after reaction
And sieving separating, respectively obtain earth solution, the insoluble sediment in platinum group metal and catalyst carrier；
(3) recovering rare earth: sodium sulphate is added to earth solution obtained in step (2), obtains sodium sulfate double salt sediment, later
Double salt of rare earth is obtained by filtration, lanthanum, cerium mixed rare-earth oxide are prepared；
(4) roasting of platinum group metal: sodium hydroxide solution will be added in platinum group metal sediment obtained in step (2), in temperature
700-800 DEG C of roasting 7-8h is spent, then leaches 30-40min, repeated calcination 2-3 times with 10 times of boiling boiling；
(5) it recycles platinum group metal: the product that step (4) obtains being passed through chlorine and is carried out at potassium cloride, separation and purifying technique
After reason, platinum group metal platinum, palladium, rhodium are obtained.
2. a kind of side of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles according to claim 1
Method, it is characterised in that: the catalyst in the step (1) passes through preheating before curing, and heating temperature is 1000-1200
DEG C, heating time 3-4h.
3. a kind of side of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles according to claim 1
Method, it is characterised in that: the mass ratio of curing material and water described in the step (2) is 1: 4.
4. a kind of side of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles according to claim 1
Method, it is characterised in that: step (4) repeated calcination is 3 times.
5. a kind of side of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles according to claim 1
Method, it is characterised in that: the concentration of the sodium hydroxide solution in the step (4) is 200-300g/L.
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| CN201910169618.3A CN109722541A (en) | 2019-02-27 | 2019-02-27 | A method of recovering rare earth and platinum group metal from failure cleaning catalyst for tail gases of automobiles |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113106258A (en) * | 2021-04-20 | 2021-07-13 | 洛阳昊海环保科技有限公司 | Method for dissolving out noble metal in waste automobile exhaust purification 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 |
| CN114606392A (en) * | 2022-03-16 | 2022-06-10 | 贵研资源（易门）有限公司 | Method for separating platinum group metal-containing coating in waste VOCs metal carrier catalyst |
| RU2802033C1 (en) * | 2023-01-17 | 2023-08-22 | Общество с ограниченной ответственностью "Промышленные технологии рециклинга" | Method for processing deactivated automobile catalysts |
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| US20040081602A1 (en) * | 2002-10-25 | 2004-04-29 | Han Kenneth N. | Recovery of platinum group metals |
| WO2005083131A1 (en) * | 2004-02-27 | 2005-09-09 | National Institute Of Advanced Industrial Science And Technology | Extractants for palladium and process for separation and recovery of palladium |
| CN103290223A (en) * | 2013-05-28 | 2013-09-11 | 北京矿冶研究总院 | Comprehensive recovery method for multiple metals of waste catalyst |
| CN103361499A (en) * | 2013-07-23 | 2013-10-23 | 昆明贵金属研究所 | Method for recovering rare earth elements from spent automobile catalyst |
| 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 |
| CN108588403A (en) * | 2018-07-27 | 2018-09-28 | 江苏北矿金属循环利用科技有限公司 | One kind is from indissoluble α-Al2O3The method that platinum is recycled in base platinum-containing waste catalyst |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20040081602A1 (en) * | 2002-10-25 | 2004-04-29 | Han Kenneth N. | Recovery of platinum group metals |
| WO2005083131A1 (en) * | 2004-02-27 | 2005-09-09 | National Institute Of Advanced Industrial Science And Technology | Extractants for palladium and process for separation and recovery of palladium |
| CN103290223A (en) * | 2013-05-28 | 2013-09-11 | 北京矿冶研究总院 | Comprehensive recovery method for multiple metals of waste catalyst |
| CN103361499A (en) * | 2013-07-23 | 2013-10-23 | 昆明贵金属研究所 | Method for recovering rare earth elements from spent automobile catalyst |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113106258A (en) * | 2021-04-20 | 2021-07-13 | 洛阳昊海环保科技有限公司 | Method for dissolving out noble metal in waste automobile exhaust purification 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 |
| CN114606392A (en) * | 2022-03-16 | 2022-06-10 | 贵研资源（易门）有限公司 | Method for separating platinum group metal-containing coating in waste VOCs metal carrier catalyst |
| RU2802033C1 (en) * | 2023-01-17 | 2023-08-22 | Общество с ограниченной ответственностью "Промышленные технологии рециклинга" | Method for processing deactivated automobile catalysts |
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