CN109680154A - A method of gold-palladium is separated and recovered from dead catalyst - Google Patents
A method of gold-palladium is separated and recovered from dead catalyst Download PDFInfo
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- CN109680154A CN109680154A CN201910121788.4A CN201910121788A CN109680154A CN 109680154 A CN109680154 A CN 109680154A CN 201910121788 A CN201910121788 A CN 201910121788A CN 109680154 A CN109680154 A CN 109680154A
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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
- C22B7/001—Dry processes
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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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- 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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- 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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Abstract
A method of gold-palladium is separated and recovered from dead catalyst.The present invention relates to the methods of a kind of separating and recovering gold, palladium from aluminium base palladium/Au catalyst.Process route is as follows: Leaching in Column at Normal Temperature → iron plate displacement enrichment gold-palladium → gold-palladium enriched substance dissolution → ferrous iron selective reduction gold → chlorination ammonia-sinking palladium → dichloro diammonium network Asia palladium purifying palladium → hydrazine hydrate reduction prepares palladium sponge.This method technique is brief, and cost recovery is low, metal high income, and palladium and gold recovery are greater than 98.5%, and purity is >=99.95%.
Description
Technical field
The invention belongs to recycle gold-palladium field, and in particular to a method of gold-palladium is separated and recovered from dead catalyst.
Background technique
Platinum group metal, resource scarcity, the content in the earth's crust only have 0.001-0.01g/t (Pt 0.005g/t), price
Valuableness also has and its important use in addition to extremely important economic value in modern science and technology and industrial development process
On the way.Platinum group metal has excellent catalytic performance.In chemical industry, especially in petro chemical industry, oil-refinery industry, doctor
In medicine and energy industry, the catalyst of platinum group metal such as platinum, palladium is widely used.For platinum, petrochemical industry (reform and
Catalytic pyrolysis), chemical fertilizer industry (synthetic ammonia catalyst) and eliminate the fields such as automobile exhaust pollution and be widely used.In addition, electronics,
The fields such as glass ceramics and military project also have highly important purposes.China platinum group metal lacks, and foreign exchange need to be spent from state every year
Outer import platinum group metal meets the needs of the development of the national economy.Thus, platinum group metal is recycled in continuous improvement from dead catalyst
Engineering and industrialization level, be particularly important.
Palladium/Au catalyst of alumina base is widely used in ethylene vapour phase oxidation process preparing vinyl acetate, generally uses 2 years or so
Catalytic activity will be lost.Recover palladium and gold from the useless Used palladium catalyst that carrier is aluminium oxide or silica, generally take
The complete insoluble only selective dissolution palladium of molten or carrier of wet process and gold, will all dissolve out a large amount of aluminium and silicon, leachate volume is big, liquid in this way
Admittedly separate it is extremely difficult, cause palladium and gold leaching rate and the rate of recovery it is not high.
Summary of the invention
It is an object of the invention to: a kind of selective dissolution palladium and gold are provided, and infusion solution amount is less, without washing
The dissolving-out method of filtering.Using the technique of Leaching in Column at Normal Temperature, eliminate filtering and washing operation, this method compared with the conventional method,
Process flow is short, equipment is simple, the amount of solution of ton dead catalyst output is few, leaching rate is high.
Technical scheme is as follows: a method of gold-palladium is separated and recovered from dead catalyst, comprising the following steps:
S1: aluminium base palladium/Au catalyst is subjected to roasting removing carbon distribution and organic matter；
S2: carrying out series connection leaching for aluminium base palladium/Au catalyst, 10~40 DEG C of temperature, leachate volume be material quantity 3~
8 times, acid concentration is 1~5mol/L；
S3: into the leachate of S2 be added iron plate displacement it is therein gold and palladium, iron plate additional amount be amount of solution 1~
10%, temperature is room temperature, and the time is 16~48h；
S4: gold-palladium substitution product in S3 is dissolved, and selecting hydrochloric acid to add, hydrogen peroxide dissolves or hydrochloric acid adds sodium chlorate, temperature 70
~100 DEG C, 2~6h of time；
S5: will be added ferrous selective reduction gold, select frerrous chloride or ferrous sulfate solution in the gold-palladium solution in S4,
Additional amount is 1.1~5 times of theoretical amount, and temperature is 50~100 DEG C, 1~5h of time；
S6: after the reduction of S5 gold, chlorination ammonia-sinking palladium is added in palladium-containing solution, to obtain chlorine palladium acid amide precipitating；
S7: the precipitating of chlorine palladium acid amide obtained by S6 is purified using dichloro diammonium network Asia palladium method, then is carried out using hydrazine hydrate
Reduction, obtains palladium sponge.
In the S1, maturing temperature is 500~700 DEG C.
In the S2, aluminium base palladium/Au catalyst is placed in 4 leaching towers, carries out series connection leaching, single column leaching at normal temperature
The time is 24~96h out.
In the S2, leaching agent be one or more of hydrochloric acid, sulfuric acid, nitric acid mixed acid, oxidant be hydrogen peroxide,
One or more of sodium chlorate, sodium hypochlorite are mixed.
In the S4, hydrochloric acid is selected to add sodium chlorate.
In the S4, aqua regia dissolution is selected.
In the S5, solution of ferrous chloride is selected.
In the S6, ammonium chloride additional amount is 2~8 times of palladium metal amount, and hydrogen peroxide or sodium chlorate oxidation, reaction is added
10~40 DEG C of temperature, the time 4~for 24 hours.
In the S7, washing sponge palladium is boiled with the analysis pure hydrochloric acid of 2mol/L, then neutrality is washed with deionized, dried,
Obtain product palladium sponge.
Remarkable result of the invention is:
1, using the technique of Leaching in Column at Normal Temperature, selective dissolution palladium and gold, without washing filtering, eliminate difficult filtering with
Washing operation.
2, process flow is short, equipment is simple, the amount of solution of ton dead catalyst output is few, palladium leaching rate and the rate of recovery are high,
Processing cost is low.
3, it is restored using ferrous iron, the reduction for the property of can choose is golden and palladium is not reduced, and simply and effectively realizes gold-palladium point
From.
Specific embodiment
Embodiment 1
A method of gold-palladium is separated and recovered from dead catalyst, comprising the following steps:
S1: carrying out roasting removing carbon distribution and organic matter for aluminium base palladium/Au catalyst first, and maturing temperature is 500~700
DEG C, avoid palladium from being oxidized；
S2: aluminium base palladium/Au catalyst is placed in 4 leaching towers, carries out series connection leaching at normal temperature, and leaching agent is salt
The mixed acid of one or more of acid, sulfuric acid, nitric acid, oxidant are one of hydrogen peroxide, sodium chlorate, sodium hypochlorite or several
Kind is mixed, and 10~40 DEG C of temperature, single column extraction time is 24~96h, and leachate volume is 3~8 times of material quantity, and acid concentration is
1~5mol/L；
S3: into the leachate of S2 be added iron plate displacement it is therein gold and palladium, iron plate additional amount be amount of solution 1~
10%, temperature is room temperature, and the time is 16~48h；
S4: gold-palladium substitution product in S3 is dissolved, and hydrochloric acid is selected to add hydrogen peroxide (or sodium chlorate), or selection chloroazotic acid (hydrochloric acid+
Nitric acid) dissolution, 70~100 DEG C of temperature, 2~6h of time；
S5: ferrous selective reduction gold will be added in the gold-palladium solution in S4, select frerrous chloride or ferrous sulfate, be added
Amount is 1.1~5 times of theoretical amount, and temperature is 50~100 DEG C, 1~5h of time；
S6: after the reduction of S5 gold, chlorination ammonia-sinking palladium is added in palladium-containing solution, to obtain chlorine palladium acid amide precipitating
Ammonium chloride additional amount is 2~8 times of palladium metal amount, and hydrogen peroxide or sodium chlorate oxidation is added, reaction temperature 10~
40 DEG C, the time 4~for 24 hours；
S7: the precipitating of chlorine palladium acid amide obtained by S6 is purified using dichloro diammonium network Asia palladium method, then is carried out using hydrazine hydrate
Reduction, obtains palladium sponge, boils washing sponge palladium with the analysis pure hydrochloric acid of 2mol/L, then neutrality is washed with deionized, and dries, obtains
To product palladium sponge.
Embodiment 2
Then plus water Pd/Au-Al2O3 dead catalyst 10kg containing Pd0.28%, Au0.25%, roasts 4h at 900 DEG C,
30 liters, with formic acid 100ml reductase 12 h, the catalyst after reduction is fitted into the glass column of Ф 100 × 1500, glass column can press from both sides
Set heating.By the HCl (the oxidant 10g/L, the promotor 30g/L that code name is B that are A containing code name) of 90 liters of 2mol/L with 20ml/
The flow velocity of min, is slowly added into glass column, flows out after catalyst bed.After 90 liters of leaching agents pass through, analysis is leached
Containing Pd in catalyst afterwards is 0.002%, Au0.001%, and Pd leaching rate is that 99.3%, Au leaching rate is 99.6%.Containing gold-palladium
Leachate with iron plate replace 24 lab scales, replace tail washings 0.3mg/L containing Pd, 0.1mg/L containing Au.By substitution product 4mol/L
Hydrochloric acid oxidizer dissolve and filter, the greening that 3 times of theoretical amounts are added in lysate containing gold-palladium is ferrous, restores 3 at 90 DEG C
Hour, filter to isolate bronze.It after bronze catches up with nitre with aqua regia dissolution, is restored with sodium sulfite, obtains the proof gold powder of 24.8g, gold
The rate of recovery be 99.2%, purity be greater than 99.95%, impurity meets national standard and petrochemical industry standard.Lysate warp containing gold-palladium
After ferrous Reduced separating gold, excessive ammonium chloride is added and oxidant generates red ammonium chloropalladate precipitating, filters and uses 50g/L
Ammonium chloride solution washing, ammonium chloropalladate after purification, obtains 26.8g palladium sponge with hydrazine hydrate reduction through dichloro diammonium network Asia palladium method
Product, direct yield 95.7%, the palladium containing 0.94g in mother liquor of precipitation of ammonium, overall recovery 99.1%.Palladium sponge purity is greater than
99.95%, impurity meets national standard and petrochemical industry standard.
Embodiment 3
A method of gold-palladium is separated and recovered from dead catalyst, comprising the following steps:
S1: carrying out roasting removing carbon distribution and organic matter for aluminium base palladium/Au catalyst first, and maturing temperature is 500 DEG C, avoids
Palladium is oxidized；
S2: aluminium base palladium/Au catalyst is placed in 4 leaching towers, carries out series connection leaching at normal temperature, and leaching agent is salt
The mixed acid of one or more of acid, sulfuric acid, nitric acid, oxidant are one of hydrogen peroxide, sodium chlorate, sodium hypochlorite or several
Kind is several mixed, and 10 DEG C of temperature, single column extraction time is that for 24 hours, leachate volume is 3 times of material quantity, acid concentration 1mol/
L；
S3: iron plate displacement gold therein and palladium being added into the leachate of S2, and iron plate additional amount is the 1% of amount of solution, temperature
Degree is room temperature, time 16h；
S4: gold-palladium substitution product in S3 is dissolved, and hydrochloric acid is selected to add hydrogen peroxide (or sodium chlorate), or selection chloroazotic acid (hydrochloric acid+
Nitric acid) dissolution, temperature 70 C, time 2h；
S5: ferrous selective reduction gold will be added in the gold-palladium solution in S4, select frerrous chloride or ferrous sulfate, be added
Amount is 1.1 times of theoretical amount, and temperature is 50 DEG C, time 1h；
S6: after the reduction of S5 gold, chlorination ammonia-sinking palladium is added in palladium-containing solution, to obtain chlorine palladium acid amide precipitating
Ammonium chloride additional amount is 2 times of palladium metal amount, and hydrogen peroxide or sodium chlorate oxidation is added, 10 DEG C of reaction temperature, when
Between 4h；
S7: the precipitating of chlorine palladium acid amide obtained by S6 is purified using dichloro diammonium network Asia palladium method, then is carried out using hydrazine hydrate
Reduction, obtains palladium sponge, boils washing sponge palladium with the analysis pure hydrochloric acid of 2mol/L, then neutrality is washed with deionized, and dries, obtains
To product palladium sponge.
Embodiment 4
A method of gold-palladium is separated and recovered from dead catalyst, comprising the following steps:
S1: carrying out roasting removing carbon distribution and organic matter for aluminium base palladium/Au catalyst first, and maturing temperature is 700 DEG C, avoids
Palladium is oxidized；
S2: aluminium base palladium/Au catalyst is placed in 4 leaching towers, carries out series connection leaching at normal temperature, and leaching agent is salt
The mixed acid of one or more of acid, sulfuric acid, nitric acid, oxidant are one of hydrogen peroxide, sodium chlorate, sodium hypochlorite or several
Kind is several mixed, and 40 DEG C of temperature, single column extraction time is 96h, and leachate volume is 8 times of material quantity, acid concentration 5mol/
L；
S3: iron plate displacement gold therein and palladium being added into the leachate of S2, and iron plate additional amount is the 10% of amount of solution, temperature
Degree is room temperature, time 48h；
S4: gold-palladium substitution product in S3 is dissolved, and hydrochloric acid is selected to add hydrogen peroxide (or sodium chlorate), or selection chloroazotic acid (hydrochloric acid+
Nitric acid) dissolution, 7100 DEG C of temperature, time 6h；
S5: ferrous selective reduction gold will be added in the gold-palladium solution in S4, select frerrous chloride or ferrous sulfate, be added
Amount is 5 times of theoretical amount, and temperature is 100 DEG C, time 5h；
S6: after the reduction of S5 gold, chlorination ammonia-sinking palladium is added in palladium-containing solution, to obtain chlorine palladium acid amide precipitating
Ammonium chloride additional amount is 8 times of palladium metal amount, and hydrogen peroxide or sodium chlorate oxidation is added, 40 DEG C of reaction temperature, when
Between for 24 hours；
S7: the precipitating of chlorine palladium acid amide obtained by S6 is purified using dichloro diammonium network Asia palladium method, then is carried out using hydrazine hydrate
Reduction, obtains palladium sponge, boils washing sponge palladium with the analysis pure hydrochloric acid of 2mol/L, then neutrality is washed with deionized, and dries, obtains
To product palladium sponge.
Embodiment 5
A method of gold-palladium is separated and recovered from dead catalyst, comprising the following steps:
S1: carrying out roasting removing carbon distribution and organic matter for aluminium base palladium/Au catalyst first, and maturing temperature is 600 DEG C, avoids
Palladium is oxidized；
S2: aluminium base palladium/Au catalyst is placed in 4 leaching towers, carries out series connection leaching at normal temperature, and leaching agent is salt
The mixed acid of one or more of acid, sulfuric acid, nitric acid, oxidant are one of hydrogen peroxide, sodium chlorate, sodium hypochlorite or several
Kind is several mixed, and 20 DEG C of temperature, single column extraction time is 36h, and leachate volume is 5 times of material quantity, acid concentration 2mol/
L；
S3: iron plate displacement gold therein and palladium being added into the leachate of S2, and iron plate additional amount is the 5% of amount of solution, temperature
Degree is room temperature, and the time is for 24 hours；
S4: gold-palladium substitution product in S3 is dissolved, and hydrochloric acid is selected to add hydrogen peroxide (or sodium chlorate), or selection chloroazotic acid (hydrochloric acid+
Nitric acid) dissolution, 80 DEG C of temperature, time 4h；
S5: ferrous selective reduction gold will be added in the gold-palladium solution in S4, select frerrous chloride or ferrous sulfate, be added
Amount is 2 times of theoretical amount, and temperature is 60 DEG C, time 2h；
S6: after the reduction of S5 gold, chlorination ammonia-sinking palladium is added in palladium-containing solution, to obtain chlorine palladium acid amide precipitating
Ammonium chloride additional amount is 4 times of palladium metal amount, and hydrogen peroxide or sodium chlorate oxidation is added, 20 DEG C of reaction temperature, when
Between 6h；
S7: the precipitating of chlorine palladium acid amide obtained by S6 is purified using dichloro diammonium network Asia palladium method, then is carried out using hydrazine hydrate
Reduction, obtains palladium sponge, boils washing sponge palladium with the analysis pure hydrochloric acid of 2mol/L, then neutrality is washed with deionized, and dries, obtains
To product palladium sponge.
Claims (9)
1. a kind of method from dead catalyst separation and recovery gold-palladium, it is characterised in that: the following steps are included: S1: by aluminium base palladium/gold
Catalyst carries out roasting removing carbon distribution and organic matter；
S2: carrying out series connection leaching for aluminium base palladium/Au catalyst, and 10~40 DEG C of temperature, leachate volume is 3~8 times of material quantity,
Acid concentration is 1~5mol/L；
S3: iron plate displacement gold therein and palladium being added into the leachate of S2, and iron plate additional amount is the 1~10% of amount of solution, temperature
Degree is room temperature, and the time is 16~48h；
S4: gold-palladium substitution product in S3 is dissolved, and selecting hydrochloric acid to add, hydrogen peroxide dissolves or hydrochloric acid adds sodium chlorate, temperature 70~100
DEG C, 2~6h of time；
S5: ferrous selective reduction gold will be added in the gold-palladium solution in S4, select frerrous chloride or ferrous sulfate solution, be added
Amount is 1.1~5 times of theoretical amount, and temperature is 50~100 DEG C, 1~5h of time；
S6: after the reduction of S5 gold, chlorination ammonia-sinking palladium is added in palladium-containing solution, to obtain chlorine palladium acid amide precipitating；
S7: the precipitating of chlorine palladium acid amide obtained by S6 being purified using dichloro diammonium network Asia palladium method, then is restored using hydrazine hydrate,
Obtain palladium sponge.
2. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 1, it is characterised in that: the S1
In, maturing temperature is 500~700 DEG C.
3. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 1, it is characterised in that: the S2
In, aluminium base palladium/Au catalyst is placed in 4 leaching towers, carries out series connection leaching at normal temperature, single column extraction time is 24~
96h。
4. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 3, it is characterised in that: the S2
In, leaching agent is the mixed acid of one or more of hydrochloric acid, sulfuric acid, nitric acid, and oxidant is hydrogen peroxide, sodium chlorate, hypochlorous acid
One or more of sodium is mixed.
5. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 1, it is characterised in that: the S4
In, select hydrochloric acid to add sodium chlorate.
6. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 1, it is characterised in that: the S4
In, select aqua regia dissolution.
7. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 1, it is characterised in that: the S5
In, select solution of ferrous chloride.
8. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 1, it is characterised in that: the S6
In, ammonium chloride additional amount is 2~8 times of palladium metal amount, and hydrogen peroxide or sodium chlorate oxidation is added, 10~40 DEG C of reaction temperature,
Time 4~for 24 hours.
9. a kind of method from dead catalyst separation and recovery gold-palladium according to claim 1, it is characterised in that: the S7
In, washing sponge palladium is boiled with the analysis pure hydrochloric acid of 2mol/L, then neutrality is washed with deionized, dries, obtain product palladium sponge.
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| CN109957659A (en) * | 2019-04-30 | 2019-07-02 | 厦门英科恒生环保咨询有限公司 | A kind of recovery method containing Used palladium catalyst |
| CN112063853A (en) * | 2020-09-01 | 2020-12-11 | 昆明铂锐金属材料有限公司 | Method for recovering palladium from spent palladium resin catalyst |
| US20210047708A1 (en) * | 2019-08-15 | 2021-02-18 | Battelle Energy Alliance, Llc | Methods of selectively recovering palladium from a palladium-containing material |
| CN114717418A (en) * | 2022-02-24 | 2022-07-08 | 阳谷祥光铜业有限公司 | Method for extracting high-purity spongy platinum from platinum waste liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109957659A (en) * | 2019-04-30 | 2019-07-02 | 厦门英科恒生环保咨询有限公司 | A kind of recovery method containing Used palladium catalyst |
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| US12012642B2 (en) * | 2019-08-15 | 2024-06-18 | Battelle Energy Alliance, Llc | Methods of selectively recovering palladium from a palladium-containing material |
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| CN114717418A (en) * | 2022-02-24 | 2022-07-08 | 阳谷祥光铜业有限公司 | Method for extracting high-purity spongy platinum from platinum waste liquid |
| CN114717418B (en) * | 2022-02-24 | 2024-02-23 | 阳谷祥光铜业有限公司 | Method for extracting high-purity sponge platinum from platinum waste liquid |
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Application publication date: 20190426 |