CN107326192A - The method that rhodium is reclaimed from auto-exhaust catalyst - Google Patents
The method that rhodium is reclaimed from auto-exhaust catalyst Download PDFInfo
- Publication number
- CN107326192A CN107326192A CN201710417960.1A CN201710417960A CN107326192A CN 107326192 A CN107326192 A CN 107326192A CN 201710417960 A CN201710417960 A CN 201710417960A CN 107326192 A CN107326192 A CN 107326192A
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- Prior art keywords
- rhodium
- reclaimed
- catalyst
- auto
- exhaust 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- 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
- C22B11/06—Chloridising
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/0015—Obtaining aluminium by wet processes
- C22B21/0023—Obtaining aluminium by wet processes from waste materials
- C22B21/003—Obtaining aluminium by wet processes 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to auto-exhaust catalyst recovery technology field, and in particular to a kind of method that rhodium is reclaimed from auto-exhaust catalyst, including：Catalyst pulverization process will be reclaimed, catalyst powder is obtained；Catalyst powder plus alkali are calcined；By the material dissolution after roasting and separation of solid and liquid processing is carried out, obtain filter residue；With hydrochloric acid and dioxygen flooding filter residue, leachate is obtained；Elution processing is carried out to resin with after resin adsorption leachate, leacheate is obtained, and rhodium will be precipitated in hydrazine hydrate addition leacheate.Compared with existing recovery technology, the leaching process of rhodium will not have poison gas generation in technical solution of the present invention, environmentally friendly, leaching rate, the rate of recovery of rhodium are high, and removal process of the present invention is simple and easy to apply, and reaction condition is easily controllable, equipment requirement and production cost are low, suitable for industrial applications.
Description
Technical field
The invention belongs to auto-exhaust catalyst recovery technology field, and in particular to one kind is returned from auto-exhaust catalyst
The method for receiving rhodium.
Background technology
To improve urban air quality, countries in the world are all being formulated and are implementing more strict automobile exhaust emission standard,
Since 1990s, platinum, palladium, rhodium ternary cleaning catalyst for tail gases of automobiles (Three Way Catalysts, TWCs) by
It is used widely the advantages of chemical property stabilization, good purification, long service life.Often set automobile catalyst platinum family is golden
Category consumption is about 1~2g, and purifying vehicle exhaust field has turned into the maximum consumer fields of platinum group metal PGM (Pt, Pd and Rh).
Cleaning catalyst for tail gases of automobiles is mainly made up of carrier, coating and active material.Carrier is generally ceramic honeycomb violet
Green stone, carrier surface applies the γ-A1 of high activity2O3Coating to increase surface area, as the precious metals pt of active component, Pd and
Rh high degree of dispersion is in the coating.
Platinum group metal is increasingly rare, expensive, especially rhodium, and 1 ton of rhodium value is at 200,000,000 dollars or so.However, existing
The recovery technology efficiency of platinum group metal is not too much high in abandoned car catalyst, and environmental issue is protruded, and mainly reclaims work
Skill is cumbersome, and scale is not mature enough, and investment is big, and cost is high.The rate of recovery of especially rhodium is relatively low, traces it to its cause mainly due to rhodium
Leaching rate it is not high.
The content of the invention
Present invention aims to overcome that the defect of prior art reclaims rhodium there is provided one kind from cleaning catalyst for tail gases of automobiles
Method, to solve the technical problem that leaching rate is not high, the rate of recovery is low of rhodium in the prior art.
To achieve the above object, the technical scheme is that, it is a kind of that rhodium is reclaimed from cleaning catalyst for tail gases of automobiles
Method, comprises the following steps：
Catalyst pulverization process will be reclaimed, catalyst powder is obtained；
Alkali is added to be calcined the catalyst powder, the operating temperature of the roasting is 400~600 DEG C, working time
For 3~4h；
By the material dissolution after the roasting and separation of solid and liquid processing is carried out, obtain filter residue；
With filter residue described in hydrochloric acid and dioxygen flooding, leachate is obtained；
With elution processing is carried out to the resin after leachate described in resin adsorption, leacheate is obtained, and hydrazine hydrate is added
Rhodium is precipitated in the leacheate.
Compared with existing recovery technology, the leaching process of rhodium will not have poison gas generation in technical solution of the present invention, to ring
Border is friendly, and leaching rate, the rate of recovery of rhodium are high, and removal process of the present invention is simple and easy to apply, and reaction condition is easily controllable, and equipment will
Production cost of summing is low, suitable for industrial applications.
Brief description of the drawings
Fig. 1 is the method flow schematic diagram of recovery rhodium in cleaning catalyst for tail gases of automobiles of the present invention.
Embodiment
In order that technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment and accompanying drawing, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used
To explain the present invention, it is not intended to limit the present invention.
As shown in Figure 1, embodiments of the invention are using the method that rhodium is reclaimed from cleaning catalyst for tail gases of automobiles, step
It is as follows：
S01：Catalyst pulverization process will be reclaimed, catalyst powder is obtained；
S02：Catalyst powder plus alkali being calcined, the operating temperature of roasting is 400~600 DEG C, the working time is 3~
4h；
S03：By the material dissolution after roasting and separation of solid and liquid processing is carried out, obtain filter residue；
S04：With hydrochloric acid and dioxygen flooding filter residue, leachate is obtained；
S05：Elution processing is carried out to resin with after resin adsorption leachate, leacheate is obtained, and hydrazine hydrate is added into elution
Rhodium is precipitated in liquid.
Leached simultaneously using hydrochloric acid and hydrogen peroxide mixed solution in the embodiment of the present invention, the leaching rate of rhodium is high, leaching process
There will not be poison gas (Cl2) produce, it is environmentally friendly, and be leaching direct to filter residue, method is simple and easy to apply, and reaction condition is easy to
Control, equipment requirement and production cost are low.And resin adsorption leachate is used, the rhodium rate of recovery is high.
Specifically, during step S01, as an embodiment, 160~250 are crossed after catalyst pulverization process by reclaiming
Mesh sieve, preferably 200 mesh sieves.Catalyst powder after mesh sieve is more beneficial for the enrichment and leaching of rhodium.
Specifically, during step S02, the alkali that roasting is added is sodium hydroxide, and catalyst powder is pressed with sodium hydroxide
Mass ratio 1:(0.6~1.4), preferably 1:When (0.9~1.1), rate of roasting can be accelerated, roasting efficiency is significantly improved.And urge
Agent powder is ground with sodium hydroxide in agate mortar, well mixed to be calcined again, is difficult to adhere on alms bowl wall.
Specifically, during step S03, material dissolution process use scheme for：It is (12 that water and material are pressed into liquid-solid ratio
~6)：1 ratio mixing, preferably liquid-solid ratio (10~8):1, stir 1~2h.This scheme can be completely dissolved the thing after roasting
Material, its technique is simple, and the used time is few.
Separation of solid and liquid processing simultaneously can use suction filtration method, and suction filtration number of times preferably 2 times, its separating rate is fast, Ke Yishi
Existing filtrate, filter residue separation are thorough, improve separative efficiency.Filtered filtrate pH value is adjusted to 3.5~4.0, Al is filtrated to get
(OH)3；Because, containing abundant aluminium, this step can further reclaim aluminium, make full use of money in filtered filtrate in the present embodiment
Source.
Specifically, during step S04, as an embodiment, using 4~7mol/L hydrochloric acid (preferably 5~6mol/L)
Hydrochloric acid and hydrogen peroxide in mixed solution, mixed solution are mixed to obtain with 1.0~1.8mol/L hydrogen peroxide (preferably 1.2~1.5mol/L)
Content (mole) than be (4~7):1, its mixed solution is (8~12) by liquid-solid ratio with filter residue after mixing:1 carries out extraction filter
Slag, the temperature of extraction is 65~85 DEG C, and the time is 2~3h.Meanwhile, 1~1.5mol/L NaCl are also contained in hydrochloric acid, to increase
Cl in solution-Concentration, further improves the leaching rate of rhodium；Hydrogen peroxide is gradually added dropwise in leaching process, to increase hydrogen peroxide
Utilization rate.Further to improve the leaching rate of rhodium, before leaching process implementation, filter residue can be first dried, drying temperature is 80~
100 DEG C, the time is 18~24h.
Specifically, during step S05, the resin used is 201 × 7 resins, can further improve the rate of recovery of rhodium；
Meanwhile, ammonium chloride is added to the residual solution after resin adsorption, ammonium chloropalladate is filtered to obtain, can be to automobile catalyst in the present embodiment
In palladium reclaimed.
In a word, under the synergy of above-mentioned steps, the leaching scheme can significantly improve the leaching rate of rhodium, now the leaching of rhodium
Extracting rate is up to more than 96%.
It is of the invention successively to carry out test of many times, now lift A partial experiment result further detailed as reference pair invention progress
Thin description, is described in detail with reference to specific embodiments and the drawings 1.
Embodiment 1
The present embodiment reclaims rhodium from abandoned car tai-gas clean-up catalyst, while Recover palladium and aluminium.Comprise the following steps：
S11：By abandoned car tai-gas clean-up catalyst attrition grinding to fine powdered, 200 mesh sieves are all crossed.
S12：By the powder after mesh sieve and sodium hydroxide according to mass ratio 1:1 is well mixed in agate mortar, Ran Hou
3h is calcined under the conditions of 400 DEG C.
S13：Material after being calcined using pure water stirring and dissolving, liquid-solid ratio 10:1, stir 1h.Suction filtration twice, obtains filtrate
And filter residue, filtrate pH value is adjusted back to 3.5, is filtrated to get Al (OH)3Precipitation, is reclaimed；Filter residue is put into baking oven under the conditions of 90 DEG C,
Dry 18h.
S14：Hydrochloric acid (concentration is 6mol/L, contains 1mol/L NaCl) and hydrogen peroxide (concentration is 1.2mol/L) are mixed
Mixed solution is obtained, the molar content ratio of hydrochloric acid and hydrogen peroxide in the platinum group metal in filter residue, mixed solution is leached with mixed solution
For 4:1；The liquid-solid ratio of leaching is 8:1, extraction temperature is 75 DEG C, and extraction time 2h is obtained after leaching containing platinum group metal palladium, rhodium
Leachate.Wherein, the leaching rate of palladium is 95%, and the leaching rate of rhodium is 96%.In addition, the feed postition of hydrogen peroxide is to leach
During be gradually added dropwise, to increase dioxygen water use efficiency.
S15：Rhodium in the leachate obtained with 201 × 7 resin adsorption step S14, elution parsing obtains rhodium-containing leacheate,
Metal rhodium is obtained with hydrazine hydrate reduction again, is reclaimed；The residual solution containing palladium adds solid ammonium chloride after to absorption, until palladium sinks completely
Form sediment, be filtrated to get pure palladium salt ammonium chloropalladate, reclaim.
Finally, the rate of recovery of palladium is 93%, and the rate of recovery of rhodium is 95%.
Embodiment 2
The present embodiment reclaims rhodium from abandoned car tai-gas clean-up catalyst, while Recover palladium and aluminium.Comprise the following steps：
S21：By abandoned car tai-gas clean-up catalyst attrition grinding to fine powdered, 160 mesh sieves are all crossed.
S22：By the powder after mesh sieve and sodium hydroxide according to mass ratio 1:1.1 are well mixed in agate mortar, afterwards
3h is calcined under the conditions of 500 DEG C.
S23：Material after being calcined using pure water stirring and dissolving alkali, liquid-solid ratio 8:1, stir 2h.Suction filtration twice, obtains filtrate
And filter residue, filtrate adjust pH value to 3.8, be filtrated to get Al (OH)3Precipitation, is reclaimed；Filter residue is put into baking oven under the conditions of 80 DEG C,
Dry 24h.
S24：By hydrochloric acid (concentration is 5mol/L, contains 1.5mol/L NaCl)) and hydrogen peroxide (concentration is 1.5mol/L) it is mixed
Mixed solution is closed to obtain, the molar content of hydrochloric acid and hydrogen peroxide in the platinum group metal in filter residue, mixed solution is leached with mixed solution
Than for 6:1, the liquid-solid ratio of leaching is 12:1, extraction temperature is 80 DEG C, and extraction time 3h is obtained containing platinum group metal after leaching
The leachate of palladium, rhodium.Wherein, palladium, the leaching rate of rhodium are 98%.In addition, the feed postition of hydrogen peroxide is in leaching process
Gradually it is added dropwise, to increase dioxygen water use efficiency.
S25：Rhodium in the leachate obtained using 201 × 7 resin adsorption step S24, elution parsing obtains rhodium-containing elution
Liquid, then metal rhodium is obtained with hydrazine hydrate reduction, reclaim；The residual solution containing palladium adds solid ammonium chloride after to absorption, until palladium is complete
Precipitation, is filtrated to get pure palladium salt ammonium chloropalladate, reclaims.
Finally, the rate of recovery of palladium is 96%, and the rate of recovery of rhodium is 97%.
Embodiment 3
The present embodiment reclaims rhodium from abandoned car tai-gas clean-up catalyst, while Recover palladium and aluminium.Comprise the following steps：
S31：By abandoned car tai-gas clean-up catalyst attrition grinding to fine powdered, 200 mesh sieves are all crossed.
S32：By abandoned car catalyst fines and sodium hydroxide according to mass ratio 1:0.9 mixes equal in agate mortar
It is even, it is calcined 4h under the conditions of 400 DEG C.
S33：Material after being calcined using pure water stirring and dissolving alkali, liquid-solid ratio 9:1, mixing time 2h.Suction filtration twice, is obtained
Filtrate and filter residue, the pH value of filtrate pull back to 4.0, are filtrated to get Al (OH)3Precipitation, reclaims aluminium；Filter residue is put into baking oven in 100
Under the conditions of DEG C, 24h is dried.
S34：By hydrochloric acid (concentration is 5.5mol/L, contains 1.3mol/L NaCl)) and hydrogen peroxide (concentration is 1.3mol/L)
Mixed solution is mixed to obtain, the content ratio of hydrochloric acid and hydrogen peroxide in the platinum group metal in filter residue, mixed solution is leached with mixed solution
For 7:1, the liquid-solid ratio of leaching is 10:1, extraction temperature is 70 DEG C, and extraction time 2.5h is obtained containing platinum group metal after leaching
The leachate of palladium, rhodium.Wherein, the leaching rate of palladium is 96%, and the leaching rate of rhodium is 97%.In addition, the feed postition of hydrogen peroxide is
Gradually it is added dropwise in leaching process, to increase dioxygen water use efficiency.
S35：Rhodium in the leachate obtained using 201 × 7 resin adsorption step S34, elution parsing obtains rhodium-containing elution
Liquid, then metal rhodium is obtained with hydrazine hydrate reduction, reclaim；The residual solution containing palladium adds solid ammonium chloride after to absorption, until palladium is complete
Precipitation, is filtrated to get pure palladium salt ammonium chloropalladate, reclaims.
Finally, palladium, rhodium the rate of recovery it is identical, be 95%.
To sum up, in technical solution of the present invention rhodium and the leaching rate of palladium, the rate of recovery is very high.And removal process letter of the present invention
Single easy, reaction condition is easily controllable, and equipment requirement and production cost are low, suitable for industrial applications.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (9)
1. a kind of method that rhodium is reclaimed from auto-exhaust catalyst, it is characterised in that comprise the following steps：
Catalyst pulverization process will be reclaimed, catalyst powder is obtained；
Alkali is added to be calcined the catalyst powder, the operating temperature of the roasting is 400~600 DEG C, the working time is 3~
4h；
By the material dissolution after the roasting and separation of solid and liquid processing is carried out, obtain filter residue；
With filter residue described in hydrochloric acid and dioxygen flooding, leachate is obtained；
With elution processing is carried out to the resin after leachate described in resin adsorption, leacheate is obtained, and hydrazine hydrate addition is described
Rhodium is precipitated in leacheate.
2. the method for rhodium is reclaimed from auto-exhaust catalyst as claimed in claim 1, it is characterised in that the alkali is hydrogen-oxygen
Change sodium, and the mass ratio 1 of the catalyst powder and the sodium hydroxide:(0.6~1.4).
3. the method for rhodium is reclaimed from auto-exhaust catalyst as claimed in claim 2, it is characterised in that the catalyst powder
The mass ratio of body and the sodium hydroxide is 1:(0.9~1.1).
4. the method for rhodium is reclaimed from auto-exhaust catalyst as claimed in claim 1, it is characterised in that the material dissolution
Process is：It is (12~6) that water and the material are pressed into liquid-solid ratio：1 ratio mixing, stirs 1~2h.
5. the method for rhodium is reclaimed from auto-exhaust catalyst as claimed in claim 4, it is characterised in that the water and described
The liquid-solid ratio ratio of material is (10~8):1.
6. the method for rhodium is reclaimed from auto-exhaust catalyst as claimed in claim 1, it is characterised in that the salt during extraction
The mol ratio (4~7) of acid and hydrogen peroxide:Behind 1, and the hydrochloric acid and hydrogen peroxide mixing with the liquid-solid ratio of the filter residue for (8~
12):1。
7. the method for rhodium is reclaimed from auto-exhaust catalyst as claimed in claim 1, it is characterised in that the temperature of the extraction
Spend for 65~85 DEG C, the time is 2~3h.
8. the method for rhodium is reclaimed from auto-exhaust catalyst as claimed in claim 1, it is characterised in that the resin is
201 × 7 resins；And/or
The also NaCl containing 1~1.5mol/L in the hydrochloric acid.
9. the method that rhodium is reclaimed from auto-exhaust catalyst as described in claim 1-8 is any, it is characterised in that further
Including,
160~250 mesh sieves are crossed after the catalyst pulverization process；And/or
The filter residue is first dried before leaching, and the operating temperature of the drying is 80~100 DEG C, and the working time is 18~24h；With/
Or
Filtrate pH value after separation of solid and liquid processing is adjusted to 3.5~4.0, Al (OH) is filtrated to get3；And/or
Ammonium chloride is added to the residual solution after the resin adsorption, ammonium chloropalladate is filtered to obtain.
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| CN201710417960.1A CN107326192A (en) | 2017-06-06 | 2017-06-06 | The method that rhodium is reclaimed from auto-exhaust catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710417960.1A CN107326192A (en) | 2017-06-06 | 2017-06-06 | The method that rhodium is reclaimed from auto-exhaust catalyst |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107641720A (en) * | 2017-08-25 | 2018-01-30 | 金川集团股份有限公司 | A kind of method of the segmentation recovery noble metal from waste liquid containing noble metal |
| CN108906137A (en) * | 2018-06-29 | 2018-11-30 | 北京科技大学 | A kind of method that noble metal waste material directly prepares catalyst |
| CN110499421A (en) * | 2019-08-22 | 2019-11-26 | 西安凯立新材料股份有限公司 | A kind of platinum group metal circular regeneration technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385545A (en) * | 2002-05-24 | 2002-12-18 | 张方宇 | Method for recovering platinum, palladium and rhodium from waste catalyst in car tail gas |
| CN102899498A (en) * | 2012-09-28 | 2013-01-30 | 昆明理工大学 | Method for leaching platinum metals from spent automobile exhaust catalyst |
-
2017
- 2017-06-06 CN CN201710417960.1A patent/CN107326192A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385545A (en) * | 2002-05-24 | 2002-12-18 | 张方宇 | Method for recovering platinum, palladium and rhodium from waste catalyst in car tail gas |
| CN102899498A (en) * | 2012-09-28 | 2013-01-30 | 昆明理工大学 | Method for leaching platinum metals from spent automobile exhaust catalyst |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107641720A (en) * | 2017-08-25 | 2018-01-30 | 金川集团股份有限公司 | A kind of method of the segmentation recovery noble metal from waste liquid containing noble metal |
| CN107641720B (en) * | 2017-08-25 | 2019-12-31 | 金川集团股份有限公司 | Method for sectionally recovering precious metals from precious metal-containing waste liquid |
| CN108906137A (en) * | 2018-06-29 | 2018-11-30 | 北京科技大学 | A kind of method that noble metal waste material directly prepares catalyst |
| CN108906137B (en) * | 2018-06-29 | 2020-09-11 | 北京科技大学 | Method for directly preparing catalyst from noble metal waste |
| CN110499421A (en) * | 2019-08-22 | 2019-11-26 | 西安凯立新材料股份有限公司 | A kind of platinum group metal circular regeneration technique |
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