CN104060095A - Method of recovering palladium from palladium-loading aluminum oxide waste catalyst - Google Patents
Method of recovering palladium from palladium-loading aluminum oxide waste catalyst Download PDFInfo
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- CN104060095A CN104060095A CN201410269689.8A CN201410269689A CN104060095A CN 104060095 A CN104060095 A CN 104060095A CN 201410269689 A CN201410269689 A CN 201410269689A CN 104060095 A CN104060095 A CN 104060095A
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- palladium
- spent catalyst
- aluminium sesquioxide
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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
Abstract
The invention discloses a method of recovering palladium from a palladium-loading aluminum oxide waste catalyst. The method comprises the following steps: (1) grinding and sulfatizing-roasting the palladium-loading aluminum oxide waste catalyst to obtain roasting slags; (2) water leaching and filtering the roasting slags to remove aluminum to obtain palladium-enriched slags, and then immersing the palladium-enriched slags by using acid liquor of diluted hydrochloric acid and sodium hypochlorite, wherein palladium is immersed into the acid liquor to a palladium extract; and (3) purifying palladium from the palladium extract. The method of recovering palladium from the palladium-loading aluminum oxide waste catalyst disclosed by the invention is simple in process and easy to operate, the use level of the acid liquor is reduced, the generated exhaust gases are few, the amount of wastewater is reduced, the palladium recovery rate is high and the purity of palladium obtained is high, so that the method has the advantages of low cost, less pollution, environmental protection and the like.
Description
Technical field
The present invention relates to a kind of method of the precious metal reclaiming from useless noble metal catalyst, particularly from carry palladium aluminium sesquioxide spent catalyst, reclaim the method for palladium.
Background technology
Along with becoming better and approaching perfection day by day of scientific and technological progress and environmental legislation, precious metal has been not limited only to manufacture ornament and play a role in economy and finance, and be applied in Industrial processes, especially aspect petrochemical process catalyzer used, be widely used.Need a large amount of replacing because the factors such as poisoning, carbon deposit, carrier structure variation, metal grain gathering or loss cause catalyzer to lose activity every year, these catalyst value are huge, must recycle.
The precious metal such as palladium, platinum, owing to having unique physics, chemical property, has important irreplaceable effect in every field.But China's palladium and platinum resource are very deficient, price is very expensive, and domestic needs increases year by year, and the 90w% of domestic needs needs import above.Meanwhile, annual China all produces the waste material that contains in a large number palladium, platinum.Because the secondary resource that contains precious metal is compared with resource for the first time, there is content high, form relative with technological process simple, the advantage such as tooling cost is low, thereby each industrially developed country of the world all takes much count of the recycling of precious metal secondary resource.In conjunction with China's national situation, the meaning that precious metal secondary resource is recycled is more great.
Current recovery method is roughly divided into pyrogenic process and the large class of wet method two.Application is hydrometallurgic recovery more widely, leaches into and in solution, forms ionic condition, then precious metal is purified out from solution by precious metal; Particularly, adopt strong acid solution that the precious metal in spent catalyst is immersed in liquid phase, thereby and then solution is purified and obtained precious metal.The palladium liquid that soaks used has following several at present: (this method is also complete molten method for chloroazotic acid, hydrochloric acid/clorox (sodium chlorate), hydrochloric acid/chlorine, hydrochloric acid/hydrogen peroxide and sulfuric acid/hydrochloric acid/clorox, carrier alundum can be dissolved, clorox makes constantly to generate chlorine in solution as oxygenant, so clorox also can change chlorine or hydrogen peroxide into sometimes).There is the shortcoming that leaches not exclusively or introduce too many base metal impurity in these methods, and solution usage quantity is large, makes follow-up filtration and purify complicatedly, and waste water treatment engineering aggravates to bring immense pressure to environment protection, is obviously not suitable for current expanding economy.
Summary of the invention
The object of the invention is to overcome existing above-mentioned deficiency in prior art, the method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst that the rate of recovery is high, acid solution usage quantity is little and environmental protection cost is low is provided.
In order to realize foregoing invention object, the invention provides following technical scheme:
The method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst, comprises the following steps:
(1) to carrying, palladium aluminium sesquioxide spent catalyst grinds, sulfurization roasting, obtains fired slags;
(2) gained fired slags, after water logging, mistake filtering aluminium, obtains palladium enrichment slag, then uses dilute hydrochloric acid and hypochlorous acid
The acid solution of sodium is soaked described palladium enrichment slag, and palladium is immersed in described acid solution, obtains palladium leach liquor;
(3) from palladium leach liquor, purify and reclaim palladium.
Grinding carrying palladium aluminium sesquioxide spent catalyst described in above-mentioned steps (1) is that described spent catalyst is ground to form to powdery, so that sulfurization roasting processing.
In above-mentioned steps (2), adding before dilute hydrochloric acid and chlorine bleach liquor, first by the spent catalyst water logging after step (1) sulfurization roasting, filter to such an extent that add again dilute hydrochloric acid and hypochlorous leaching palladium after filter residue.
The above-mentioned method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst, specifically comprises the following steps:
1. grind: will carry palladium aluminium sesquioxide spent catalyst and pour ball mill into, ball milling 1～4h;
2. sulfurization roasting: by the spent catalyst powder vitriol oil furnishing pulpous state after grinding, be placed in rotary kiln, 550-700 DEG C of roasting 5-7h;
3. water logging: the catalyzer after roasting is dropped in reactor, add water in reactor, unlatching is stirred and is heated to temperature and reaches 60 DEG C, and constant temperature leaches 1～3h, cooling;
4. filter: filter to obtain main component be Tai-Ace S 150 filtrate and palladium enrichment slag;
5. chloric acid leaches: adopt dilute hydrochloric acid and chlorine bleach liquor to step 4. gained palladium enrichment slag leach, in leaching process, need heat and stir, Heating temperature is 90～100 DEG C, and chlorine bleach liquor adopts dropping mode slowly to add in described palladium enrichment slag, extraction time 4～6h;
6. filter: filtration step is infusion solution 5., obtains containing the expensive liquid of palladium;
7. separating-purifying: obtain High Purity Palladium powder to carrying out separating-purifying containing the expensive liquid of palladium.
Above-mentioned steps 5. in the concentration preferably 20%～30% of dilute hydrochloric acid; The volumetric usage of described dilute hydrochloric acid is preferably 1.5-2.5:1 (mL:g) with the ratio of palladium enrichment slag weight; More preferably 2:1 (mL:g).
The solution that above-mentioned chlorine bleach liquor's preferred concentration is 8% also adopts dropping mode to add in described palladium enrichment slag, drips until Leaching reaction stops front 1h always.
Above-mentioned steps 2. middle roasting condition is preferably in rotary kiln, 600 DEG C of roasting 6h.
Above-mentioned steps is described separating-purifying 7., can take dichloro diamino palladium complexometry or organic solvent extractionprocess repeatedly.
Sodium chlorate solution's described in the invention concentration, the concentration of hydrochloric acid, all refer to mass percentage concentration.
Compared with prior art, beneficial effect of the present invention: the present invention reclaims the method for palladium from carry palladium aluminium sesquioxide spent catalyst, technique is simple to operation, reduce acid solution usage quantity, the waste gas producing is less, and wastewater flow rate reduces, and palladium recovery rate is high, gained palladium purity is high, have cost low, pollute the advantages such as little, environmental protection.
Embodiment
Below in conjunction with test example and embodiment, the present invention is described in further detail.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on content of the present invention all belong to scope of the present invention.
Embodiment 1 reclaims the method for palladium from carry palladium aluminium sesquioxide spent catalyst
20Kg is carried to palladium aluminium sesquioxide spent catalyst (palladium content is 0.3%) and be placed in ball mill ball milling 1h, then by the spent catalyst powder after ball milling and vitriol oil furnishing pulpous state, be placed in 600 DEG C, rotary kiln and burn 6h.Be transferred to after cooling in 50L enamel reaction still, add the tap water of 3 times of amounts, stir water logging 2h at 60 DEG C.Then filter, filtrate collection stores in order to selling (can make water scavengine agent sells) outward, and filter residue enters subsequent processing.Filter residue (amount is greatly about 5kg left and right) is transferred in 50L enamel reaction still, adds 10L 25% HCl, stir and be heated to 92 DEG C, then start to drip 8% chlorine bleach liquor, after 3h, stop dripping chlorine bleach liquor, continue after stirring reaction 1h, stop stirring.In the time that solution is cooled to below 45 DEG C, carry out filter operation, must be containing the expensive liquid of palladium and a little filter residue.To purifying containing the expensive liquid of palladium, method of purification adopts dichloro diamino palladium complexometry repeatedly, and can obtain purity content is 99.9% High Purity Palladium powder, and the rate of recovery is 98%.
Year palladium aluminium sesquioxide waste catalyst recovery palladium that it is 0.1%～1% that the example method is equally applicable to from palladium content.
Embodiment 2 reclaims the method for palladium from carry palladium aluminium sesquioxide spent catalyst
25Kg is carried to palladium aluminium sesquioxide spent catalyst (palladium content is 0.5%) and be placed in ball mill ball milling 2h, then by the spent catalyst powder after ball milling and vitriol oil furnishing pulpous state, be placed in 650 DEG C, rotary kiln and burn 6h.Be transferred to after cooling in 10L enamel reaction still, add the tap water of 3 times of amounts, stir water logging 2.5h under 60 degrees Celsius.Then filter, filtrate collection stores in order to selling outward, and filter residue enters subsequent processing.Filter residue (amount is greatly about 6kg left and right) is transferred in 50L enamel reaction still, adds 10L 30% HCl, stir and be heated to 95 DEG C, then start to drip 8% chlorine bleach liquor, after 3.5h, stop dripping chlorine bleach liquor, continue after stirring reaction 1h, stop stirring.In the time that solution is cooled to below 45 DEG C, carry out filter operation, must be containing the expensive liquid of palladium and a little filter residue.To purifying containing the expensive liquid of palladium, method of purification is organic reagent extracting and separating, and can obtain purity content is 99.95% High Purity Palladium powder, and the rate of recovery is 98.5%.
Embodiment 3 reclaims the method for palladium from carry palladium aluminium sesquioxide spent catalyst
30Kg is carried to palladium aluminium sesquioxide spent catalyst (palladium content is 1%) and be placed in ball mill ball milling 4h, then by the spent catalyst powder after ball milling and vitriol oil furnishing pulpous state, be placed in 600 DEG C, rotary kiln and burn 6h.Be transferred to after cooling in 100L enamel reaction still, add the tap water of 3 times of amounts, stir water logging 3h at 60 DEG C.Then filter, filtrate collection stores in order to selling outward, and filter residue enters subsequent processing.Filter residue (amount is greatly about 6.5kg left and right) is transferred in 50L enamel reaction still, adds 15L 30% HCl, stir and be heated to 100 DEG C, then start to drip 8% chlorine bleach liquor, after 4h, stop dripping chlorine bleach liquor, continue after stirring reaction 1h, stop stirring.In the time that solution is cooled to below 45 DEG C, carry out filter operation, must be containing the expensive liquid of palladium and a little filter residue.To purifying containing the expensive liquid of palladium, method of purification adopts dichloro diamino palladium complexometry repeatedly, and can obtain purity content is 99.95% High Purity Palladium powder, and the rate of recovery is 99%.
Claims (7)
1. the method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst, is characterized in that, comprises the following steps:
(1) to carrying, palladium aluminium sesquioxide spent catalyst grinds, sulfurization roasting, obtains fired slags;
(2) gained fired slags, after water logging, mistake filtering aluminium, obtains palladium enrichment slag, then uses dilute hydrochloric acid and hypochlorous acid
The acid solution of sodium is soaked described palladium enrichment slag, and palladium is immersed in described acid solution, obtains palladium leach liquor;
(3) from palladium leach liquor, purify and reclaim palladium.
2. the method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst according to claim 1, it is characterized in that, grinding carrying palladium aluminium sesquioxide spent catalyst described in step (1) is that described spent catalyst is ground to form to powdery, so that sulfurization roasting processing.
3. the method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst according to claim 1 and 2, is characterized in that, specifically comprises the following steps:
1. grind: will carry palladium aluminium sesquioxide spent catalyst and pour ball mill into, ball milling 1～4h;
2. sulfurization roasting: by the spent catalyst powder vitriol oil furnishing pulpous state after grinding, be placed in rotary kiln, 550-700 DEG C of roasting 5-7h;
3. water logging: the catalyzer after roasting is dropped in reactor, add water in reactor, unlatching is stirred and is heated to temperature and reaches 60 DEG C, and constant temperature leaches 1～3h, cooling;
4. filter: filter to obtain main component be Tai-Ace S 150 filtrate and palladium enrichment slag;
5. chloric acid leaches: adopt dilute hydrochloric acid and chlorine bleach liquor to step 4. gained palladium enrichment slag leach, in leaching process, need heat and stir, Heating temperature is 90～100 DEG C, and chlorine bleach liquor adopts dropping mode slowly to add in described palladium enrichment slag, extraction time 4～6h;
6. filter: filtration step is infusion solution 5., obtains containing the expensive liquid of palladium;
7. separating-purifying: obtain High Purity Palladium powder to carrying out separating-purifying containing the expensive liquid of palladium.
4. the method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst according to claim 3, is characterized in that, step 2. middle roasting condition is in rotary kiln, 600 DEG C of roasting 6h.
5. the method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst according to claim 3, it is characterized in that, the step 5. concentration of middle dilute hydrochloric acid is 20%～30%, and the volumetric usage of described dilute hydrochloric acid is 1.5～2.5:1 (mL:g) with the ratio of palladium enrichment slag weight.
6. according to claim 4ly it is characterized in that from carrying the method that reclaims palladium palladium aluminium sesquioxide spent catalyst, step 5. described in the volumetric usage of dilute hydrochloric acid be 2:1 (mL:g) with the ratio of palladium enrichment slag weight.
7. the method that reclaims palladium from carry palladium aluminium sesquioxide spent catalyst according to claim 3, it is characterized in that, step 5. described in chlorine bleach liquor for the concentration solution that is 10% and adopt dropping mode to add in described palladium enrichment slag, drip always until acid-leaching reaction stop before 1h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988319A (en) * | 2015-06-19 | 2015-10-21 | 徐州浩通新材料科技股份有限公司 | Method and system for treating load type palladium-contained dead catalyst |
| CN107523692A (en) * | 2017-08-25 | 2017-12-29 | 金川集团股份有限公司 | A kind of acidleach drop aluminium technique of high alumina failure tail-gas catalyst |
| CN108026608A (en) * | 2015-04-21 | 2018-05-11 | 萨斯喀彻温大学 | The method of Selectively leaching and extraction noble metal in organic solvent |
| CN108265180A (en) * | 2017-12-28 | 2018-07-10 | 核工业北京化工冶金研究院 | The leaching method of platinum, palladium, rhodium in useless three-way catalyst |
| CN108425014A (en) * | 2018-03-05 | 2018-08-21 | 河南能源化工集团研究总院有限公司 | A method of extracting high pure metal palladium from useless palladium-aluminium oxide catalyst |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108026608A (en) * | 2015-04-21 | 2018-05-11 | 萨斯喀彻温大学 | The method of Selectively leaching and extraction noble metal in organic solvent |
| CN108026608B (en) * | 2015-04-21 | 2021-10-22 | 艾克希尔工厂公司 | Method for selective leaching and extraction of precious metals in organic solvents |
| CN113969358A (en) * | 2015-04-21 | 2022-01-25 | 艾克希尔工厂公司 | Method for selective leaching and extraction of precious metals in organic solvents |
| US11408053B2 (en) | 2015-04-21 | 2022-08-09 | Excir Works Corp. | Methods for selective leaching and extraction of precious metals in organic solvents |
| US11427886B2 (en) | 2015-04-21 | 2022-08-30 | Excir Works Corp. | Methods for simultaneous leaching and extraction of precious metals |
| CN113969358B (en) * | 2015-04-21 | 2023-10-20 | 艾克希尔工厂公司 | Method for selectively leaching and extracting noble metals in organic solvents |
| US11814698B2 (en) | 2015-04-21 | 2023-11-14 | Excir Works Corp. | Methods for simultaneous leaching and extraction of precious metals |
| CN104988319A (en) * | 2015-06-19 | 2015-10-21 | 徐州浩通新材料科技股份有限公司 | Method and system for treating load type palladium-contained dead catalyst |
| CN107523692A (en) * | 2017-08-25 | 2017-12-29 | 金川集团股份有限公司 | A kind of acidleach drop aluminium technique of high alumina failure tail-gas catalyst |
| CN108265180A (en) * | 2017-12-28 | 2018-07-10 | 核工业北京化工冶金研究院 | The leaching method of platinum, palladium, rhodium in useless three-way catalyst |
| CN108425014A (en) * | 2018-03-05 | 2018-08-21 | 河南能源化工集团研究总院有限公司 | A method of extracting high pure metal palladium from useless palladium-aluminium oxide catalyst |
| CN108425014B (en) * | 2018-03-05 | 2019-05-31 | 河南能源化工集团研究总院有限公司 | A method of extracting high pure metal palladium from useless palladium-aluminium oxide catalyst |
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Application publication date: 20140924 |