CN109022794A - The recovery process and device of noble metal in a kind of dead catalyst - Google Patents
The recovery process and device of noble metal in a kind of dead catalyst Download PDFInfo
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- CN109022794A CN109022794A CN201810656335.7A CN201810656335A CN109022794A CN 109022794 A CN109022794 A CN 109022794A CN 201810656335 A CN201810656335 A CN 201810656335A CN 109022794 A CN109022794 A CN 109022794A
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- dead catalyst
- reaction kettle
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- 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
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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 present invention provides the recovery process and device of noble metal in a kind of dead catalyst, and the recovery process of noble metal is that liquid phase dead catalyst is directly aoxidized to separation in strong acidic environment using hydrogen peroxide in a kind of dead catalyst, to recycle Noble Metal Rhodium；The recyclable device of noble metal in a kind of dead catalyst includes reaction kettle, dead catalyst solution inlet port pipeline, hydrogen peroxide inlet line, sulfuric acid inlet line, reaction kettle top exit pipeline, reactor bottom outlet line, reacting kettle jacketing, phase separator, incineration system, concentration systems, catalyst production process, head tank, condenser, water seal tank, peculiar smell recovery system, steam inlet pipeline, steam (vapor) outlet pipeline, desalted water inlet line；Sufficiently, overall process total time-consuming 5-10h, the rate of recovery reaches 95-98% for easy to operate, reaction.
Description
Technical field
The present invention relates to noble metal recycling field, in particular to the recovery process and dress of Noble Metal Rhodium in a kind of dead catalyst
It sets.
Technical background
Rhodium-containing catalyst prepares acetic acid in Methanol Carbonylation, is all widely used in hydroformylation of olefin, due to rhodita (-te)
Category is expensive rare metal, catalyst in use can continuous aging, if do not recycled in aging catalyst
Noble Metal Rhodium, then cause the loss of Noble Metal Rhodium, therefore, it is necessary to solve asking for the Noble Metal Rhodium recycling in aging catalyst
Topic.Patent CN148522 describes a kind of method that noble metal is recycled from dead catalyst, with hydrogen peroxide, hydrogen ion, chloride ion
Solution mixing carries out leaching pretreated catalyst, is present in noble metal component in mixed solution with ionic condition, finally
Precious metal solution is handled, noble metal is recycled.Mainly for Pt, Pd catalyst, only leach the step time is up to the method
12h, and need to require greatly to roast because handling to solid state, locate by catalyst from liquid condition processing to solid elemental stage
Reason process is complicated laborious.
Summary of the invention
To overcome above-mentioned deficiency, an object of the present invention is to provide a kind of recycling work of Noble Metal Rhodium in dead catalyst
Liquid phase dead catalyst is directly aoxidized separation using hydrogen peroxide, to recycle Noble Metal Rhodium by skill in strong acidic environment.
To achieve the goals above, the technical solution of the present invention is as follows:
The recovery process of Noble Metal Rhodium in a kind of dead catalyst proposed by the present invention, the specific steps are as follows:
(1) it aoxidizes the initial gross separation stage: the dead catalyst solution pump of certain volume being squeezed into reaction kettle, while stirring
98% sulfuric acid is added into reaction kettle, is to slowly warm up to 30~40 DEG C, hydrogen peroxide is then added into reaction kettle, keeps the temperature 2~3h,
At this point, Noble Metal Rhodium is sufficiently separated with its ligand, Noble Metal Rhodium enters water phase, ligand enters oily phase, reacts the gas warp of generation
The processing of peculiar smell recovery system is sent to after cooling.
Further, 98% sulfuric acid volume is the 10%~20% of dead catalyst liquor capacity.
Further, speed control is added in 1~1.5L/s in 98% sulfuric acid.
Further, mixing speed control is in 60-80r/min.
Further, dioxygen water volume is respectively the 30%~50% of dead catalyst liquor capacity.
Further, hydrogen peroxide concentration 25-30wt.%.
Further, speed control is added in 0.8~1.2L/s in hydrogen peroxide.
Further, mixing speed control is in 60-80r/min.
Further, temperature of reaction kettle is 90 DEG C~120 DEG C.
Further, temperature of reaction kettle is controlled by adjusting the intake of reacting kettle jacketing steam.
Further, over temperature interlock system is arranged in reaction kettle, and interlocking value is 120 DEG C, is such as higher than interlocking value, closes dioxygen
Water, steam feed valve open desalted water feeding line, system cooling, it is ensured that oxidation reaction is safe and reliable.
Further, reactor pressure is 0~0.1MPa.
Further, superpressure interlock system is arranged in reaction kettle, and interlocking value 0.1MPa is such as higher than interlocking value, closes double
Oxygen water, steam feed valve open desalted water feeding line, system decrease temperature and pressure, it is ensured that oxidation reaction is safe and reliable.
Further, reacting the gas of generation, to enter condenser after head tank buffers cooling, the liquid condensed out into
Enter water seal, a small amount of on-condensible gas enters peculiar smell recovery system.
Further, oxygen on-line monitoring system is set, when oxygen concentration reaches 5%, closes hydrogen peroxide, steam feed valve
Door opens desalted water feeding line, system cooling, it is ensured that oxidation reaction is safe and reliable.
(2) it aoxidizes the idetified separation stage: hydrogen peroxide being added with the speed of 0.8~1.2L/s and is allowed to continue to react, keeps the temperature 2h
~3h.
Further, the volume that hydrogen peroxide is added is the 40%~60% of dead catalyst liquor capacity.
Further, hydrogen peroxide concentration 25-30wt.%.
Further, mixing speed control is in 60-80r/min.
(3) the sampling analysis stage: rhodium content in sample detection oil phase squeezes into dead catalyst solution if being less than 5ppm
The static 30-50min of phase separator carries out extraction and separation；If rhodium content is greater than 5ppm in oily phase, adds hydrogen peroxide and repeat to walk
Suddenly (2) make its fully reacting, until qualified.
(4) the concentration and recovery stage: mutually sending oil to incineration system after the completion of extraction, and water phase is sent to concentration systems to be concentrated and be removed
Excessive moisture is then sent to catalyst production process production raw catelyst.
The second object of the present invention is to provide a kind of device for realizing above-mentioned technique, including reaction kettle, phase separator, a high position
Slot, the reaction kettle side wall successively open up sulfuric acid, hydrogen peroxide, dead catalyst solution inlet port, the sulphur of the reaction kettle from top to bottom
Acid, hydrogen peroxide, dead catalyst solution inlet port are sequentially connected sulfuric acid, hydrogen peroxide, dead catalyst solution pipeline, the gas at the top of reaction kettle
Mutually outlet is sequentially connected head tank, condenser, water seal tank, the import connection of gaseous phase outlet and head tank at the top of reaction kettle, high
The outlet of position slot and the import of condenser connect, and condensator outlet is connect with water seal tank, water seal tank outlet and peculiar smell recovery system
Connection, the liquid-phase outlet of reactor bottom are connect with phase separator import, mutually outlet and the incineration system import of the oil of phase separator
The water phase outlet of connection, phase separator is connect with concentration systems import, and concentration systems outlet connects with the import of catalyst production process
It connects.
The invention has the benefit that
1, operation of the present invention is simple, reaction is abundant, and overall process total time-consuming 5-10h, the rate of recovery reaches 95-98%.
2, the present invention is provided with safety interlock control system, realizes automation control, and it is horizontal to improve device essential safety.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the structural schematic diagram of the recyclable device of noble metal in this dead catalyst.
Wherein, 1, reaction kettle, 2, dead catalyst solution inlet port pipeline, 3, hydrogen peroxide inlet line, 4, sulfuric acid inlet line,
5, reaction kettle top exit pipeline, 6, reactor bottom outlet line, 7, reacting kettle jacketing, 8, phase separator, 9, incineration system,
10, concentration systems, 11, catalyst production process, 12, head tank, 13, condenser, 14, water seal tank, 15, peculiar smell recovery system,
16, steam inlet pipeline, 17, steam (vapor) outlet pipeline, 18, desalted water inlet line.
Concrete technology is shown in following embodiment.
Embodiment 1:
Methanol Carbonylation prepare the 20L solution containing dead catalyst generated during acetic acid first with pump through dead catalyst solution into
Mouth pipeline 2 is squeezed into reaction kettle 1, is then added while stirring from sulfuric acid inlet line 4 into reaction kettle 1 with the speed of 1.2L/s
98% sulfuric acid 3L, open steam inlet pipeline 16, steam is passed through into reacting kettle jacketing, is to slowly warm up to 32 DEG C, then with
20L 27.5wt.% hydrogen peroxide is added into reaction kettle 1 from hydrogen peroxide inlet line 3 for the speed of 0.9L/s, while passing through control
Steam intake in reacting kettle jacketing 7 stablizes temperature of reaction kettle at 100 DEG C.
After keeping the temperature 2.3h, then 8.5L is added into reaction kettle 1 from hydrogen peroxide inlet line 3 with the speed of 0.9L/s
27.5wt.% hydrogen peroxide is allowed to continue to react, and keeps the temperature 2.5h, and rhodium content is 4ppm in sample detection oil phase, and sample passes will be located
Dead catalyst solution after reason is squeezed into from reactor bottom outlet line 6 carries out extraction and separation in phase separator 8, extraction time is
40min mutually send oil to incineration system 9 after the completion of extraction, and water phase, which is sent, carries out concentration removing excessive moisture into concentration systems 10,
It is then sent to catalyst production process 11 and makes raw catelyst.
The gas generated in reaction process enters condenser after the buffering of head tank 12 by reaction kettle top exit pipeline 5
13, water seal tank 14 is entered after condensing, remaining a small amount of gas enters peculiar smell recovery system 15.
It is computed, the Noble Metal Rhodium rate of recovery is 96%.
Embodiment 2:
The 50L solution containing dead catalyst generated during in hydroformylation of olefin is first with pump through dead catalyst solution
Inlet line 2 is squeezed into reaction kettle 1, is then added while stirring from sulfuric acid inlet line 4 into reaction kettle 1 with the speed of 1.3L/s
Enter 98% sulfuric acid 8L, open steam inlet pipeline 16, steam is passed through into reacting kettle jacketing, is to slowly warm up to 35 DEG C, then with
20L 29.5wt.% hydrogen peroxide is added into reaction kettle 1 from hydrogen peroxide inlet line 3 for the speed of 1.0L/s, while passing through control
Steam intake in reacting kettle jacketing 7 stablizes temperature of reaction kettle at 110 DEG C.
After keeping the temperature 2.5h, then 25L is added into reaction kettle 1 from hydrogen peroxide inlet line 3 with the speed of 1L/s
29.5wt.% hydrogen peroxide is allowed to continue to react, and keeps the temperature 2.6h, and rhodium content is 3ppm in sample detection oil phase, and sample passes will be located
Dead catalyst solution after reason is squeezed into from reactor bottom outlet line 6 carries out extraction and separation in phase separator 8, extraction time is
50min mutually send oil to incineration system 9 after the completion of extraction, and water phase, which is sent, carries out concentration removing excessive moisture into concentration systems 10,
It is then sent to catalyst production process 11 and makes raw catelyst.
The gas generated in reaction process enters condenser after the buffering of head tank 12 by reaction kettle top exit pipeline 5
13, water seal tank 14 is entered after condensing, remaining a small amount of gas enters peculiar smell recovery system 15.
It is computed, the Noble Metal Rhodium rate of recovery is 98%.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (5)
1. the recovery process and device of noble metal in a kind of dead catalyst, it is characterised in that: including reaction kettle, phase separator, height
Position slot, the reaction kettle side wall successively open up sulfuric acid, hydrogen peroxide, dead catalyst solution inlet port from top to bottom, the reaction kettle
Sulfuric acid, hydrogen peroxide, dead catalyst solution inlet port are sequentially connected sulfuric acid, hydrogen peroxide, dead catalyst solution pipeline, at the top of reaction kettle
Gaseous phase outlet is sequentially connected head tank, condenser, water seal tank, the import connection of gaseous phase outlet and head tank at the top of reaction kettle,
The outlet of head tank and the import of condenser connect, and condensator outlet is connect with water seal tank, and water seal tank outlet is with peculiar smell recycling
System connection, the liquid-phase outlet of reactor bottom connect with phase separator import, the oil phase of phase separator export and incineration system into
The water phase outlet of mouth connection, phase separator is connect with concentration systems import, concentration systems outlet and the import of catalyst production process
Connection.
2. the recovery process and device of noble metal in a kind of dead catalyst according to claim 1, it is characterised in that: specific
Processing step are as follows:
(1) it aoxidizes the initial gross separation stage: the dead catalyst solution pump of certain volume being squeezed into reaction kettle, while stirring to anti-
It answers and 98% sulfuric acid is added in kettle, be to slowly warm up to 30~40 DEG C, hydrogen peroxide is then added into reaction kettle, keep the temperature 2~3h, this
When, Noble Metal Rhodium is sufficiently separated with its ligand, and Noble Metal Rhodium enters water phase, ligand enters oily phase, reacts the gas of generation through cold
But it is sent to the processing of peculiar smell recovery system afterwards；
(2) it aoxidizes the idetified separation stage: hydrogen peroxide being added with the speed of 0.8~1.2L/s and is allowed to continue to react, keeps the temperature 2h~3h；
(3) the sampling analysis stage: dead catalyst solution is squeezed into phase point if being less than 5ppm by rhodium content in sample detection oil phase
30-50min static from device carries out extraction and separation；If rhodium content is greater than 5ppm in oily phase, adds hydrogen peroxide and repeat step
(2), make its fully reacting, until qualified；
(4) the concentration and recovery stage: mutually sending oil to incineration system after the completion of extraction, and water phase is sent extra to concentration systems concentration removing
Moisture is then sent to catalyst production process production raw catelyst.
3. the recovery process and device of noble metal in a kind of dead catalyst according to claim 2, it is characterized in that step (1)
In 98% sulfuric acid volume be that speed control is added in 1~1.5L/s in 10%~20%, 98% sulfuric acid of dead catalyst liquor capacity,
Mixing speed is controlled in 60-80r/min；Dioxygen water volume is respectively the 30~50% of dead catalyst liquor capacity, and hydrogen peroxide is dense
Degree is 25~30wt.%, and speed control is added in 0.8~1.2L/s in hydrogen peroxide, and mixing speed is controlled in 60-80r/min；Reaction
Kettle temperature degree is 90 DEG C~120 DEG C, and reactor pressure is 0~0.1MPa.
4. the recovery process and device of noble metal in a kind of dead catalyst according to claim 2, it is characterized in that step (1)
Over temperature interlock system is arranged in middle reaction kettle, and interlocking value is 120 DEG C, is such as higher than interlocking value, closes hydrogen peroxide, steam feed valve,
Open desalted water feeding line；Superpressure interlock system is arranged in reaction kettle, and interlocking value 0.1MPa is such as higher than interlocking value, closes double
Oxygen water, steam feed valve open desalted water feeding line.
5. the recovery process and device of noble metal in a kind of dead catalyst according to claim 2, it is characterized in that step (1)
Oxygen on-line monitoring system is arranged in middle reaction kettle, when oxygen concentration reaches 5%, closes hydrogen peroxide, steam feed valve, opens de-
Brine feed pipeline.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810656335.7A CN109022794B (en) | 2018-06-24 | 2018-06-24 | Process and device for recovering precious metals in waste catalyst |
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| CN201810656335.7A CN109022794B (en) | 2018-06-24 | 2018-06-24 | Process and device for recovering precious metals in waste catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462900A (en) * | 2021-07-04 | 2021-10-01 | 贵研资源（易门）有限公司 | Method for recovering rhodium from waste rhodium park catalyst |
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| CN106435197A (en) * | 2016-12-09 | 2017-02-22 | 武汉凯迪电力环保有限公司 | Process and device for alkaline extraction and recovery from waste catalysts in SCR (selective catalytic reduction) denitrification |
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| CN1184858A (en) * | 1996-12-13 | 1998-06-17 | 抚顺石油化工公司洗涤剂化工厂 | Method for recovering cobalt from cobalt contg. waste catalyst used is carbonylation syntehsizing process |
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| JP2018070978A (en) * | 2016-11-02 | 2018-05-10 | 住友金属鉱山株式会社 | Recovery method of high quality rhodium powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113462900A (en) * | 2021-07-04 | 2021-10-01 | 贵研资源（易门）有限公司 | Method for recovering rhodium from waste rhodium park catalyst |
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