CN107663583A - A kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste - Google Patents
A kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste Download PDFInfo
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- CN107663583A CN107663583A CN201610615841.2A CN201610615841A CN107663583A CN 107663583 A CN107663583 A CN 107663583A CN 201610615841 A CN201610615841 A CN 201610615841A CN 107663583 A CN107663583 A CN 107663583A
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- palladium
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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 invention provides a kind of method that precious metal palladium is reclaimed from useless palladium hybrid solid chemical waste.This method includes calcination carbon removal, the molten suction filtration of acid, and regulation pH is filtered, the step such as reduction.The inventive method is simple to operation, and raw material is easy to get, and cost recovery is low, green, and palladium recovery rate is more than 99%.
Description
Technical field
The present invention be on it is a kind of from useless palladium hybrid solid chemical waste reclaim Metal Palladium method, belong to heavy metal recovery with
Recycling field.
Background technology
Palladium charcoal is a kind of important catalyst, it be widely used in the reduction of nitro, the reduction of carbon-carbon double bond, the sloughing of benzyl,
In some chemical reactions such as the hydrogenolysis of carbonyl, the disengaging of fragrant halogen, preparation of hydrogenated rosin.Palladium charcoal is also thus substantial amounts of to be used
In fine chemistry industry, pharmaceuticals industry and petroleum industry.Palladium charcoal can lose activity after being used for multiple times, and palladium therein is a kind of
Important noble metal, recycling is carried out to it can effectively avoid environmental pollution, save production cost.
Palladium dydroxide also serves as a kind of presence of form of palladium catalyst, and its catalytic activity is better than palladium charcoal, can typically use palladium charcoal to be catalyzed
Reaction, can also use palladium dydroxide.Because the catalytic activity of palladium charcoal is inadequate, changing palladium dydroxide into just can smoothly enter for some reactions
OK.Some fine chemistry industry companies, medicine intermediate company, both palladium catalysts are often had, and two after use
Kind palladium catalyst puts together processing.It is to be necessary that thus how research reclaims Metal Palladium from useless palladium hybrid solid chemical waste
's.
The method for the Recover palladium from useless palladium charcoal is reported many at present, but the research for give up palladium charcoal and palladium dydroxide is not
A lot.The method of Recover palladium mainly has two kinds of common methods of pyrogenic process and wet method from useless palladium charcoal, and they have, and pollution is big, consumes energy
Greatly, using trouble, the features such as rate of recovery of palladium is low.
The content of the invention
The present invention proposes a kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste, and the method overcomes routine
Method pollution is big, and power consumption is big, the characteristics of using trouble.Small laboratory Recover palladium is not only suitable for, environmental pollution is avoided, also is adapted for
Metal Palladium is reclaimed in chemical plant, is recycled, reduced cost.
The technical solution adopted for the present invention to solve the technical problems comprises the following steps：
Step 1: calcination carbon removal：
By the discarded object containing palladium at 500-900 DEG C calcination 3-6 hours；
Step 2: acid is molten to remove solid impurity：
The solid matter obtained after toward calcination is added in the nitric acid that mass concentration is 45-65%, solid-to-liquid ratio 1：7-9, at 60-90 DEG C
Filtered after lower boiling 3-6 hours, rinse filter residue, merging filtrate and flushing liquor；
Step 3: regulation pH：
Room temperature is controlled, with inorganic salt solution by near the amalgamation liquid regulation pH to 6.5 in step 2, is gradually added into saturated aqueous common salt,
Untill solid separates out, suction filtration obtains solid palladium salt；
Step 4: the reduction of palladium salt：
The solid palladium salt obtained in step 3 is added in deionized water, solid-to-liquid ratio 1：1, hydrazine hydrate solution is added dropwise at 70 DEG C,
When yellow is no longer shown in thing to be mixed, mixture is filtered, is dried to obtain black powder palladium sponge.
Further, a kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste, chemical solids discarded object is useless
One or both of palladium charcoal and palladium dydroxide.
Further, a kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste, dead palladium catalyst calcination temperature
For 500-900 DEG C.
Further, a kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste, it is nitric acid that acid, which boils acid used,
Its mass concentration is 45% to 65%, and it is 60-90 DEG C that acid, which boils temperature used, and it is 3-6 hours that acid, which boils the time used,.
Further, a kind of method for reclaiming Metal Palladium from useless palladium hybrid solid chemical waste, adjust pH to 6.5 used nearby
Inorganic salts are sodium acid carbonate, saleratus, sodium carbonate, one kind in potassium carbonate, and adjusting needs to control room temperature, institute during pH
It is saturated aqueous common salt with saline solution.
Further, a kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste, institute's amount of water is palladium salt quality
One times, the weight of added hydrazine hydrate is 6-10 times of palladium salt.
The invention provides a kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste, raw material is cheap and easy to get, behaviour
Make simple, rate of recovery height.Laboratory is not only suitable for for same solid mixture system to reclaim in a small amount, and it is a large amount of to be also applied for factory
Recycle.
Embodiment
The scheme that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste of the present invention is further described below, made
Those skilled in the art can be better understood by and utilize the present invention
Embodiment 1
1000g is given up palladium solid mixture, wherein 15g containing palladium, is put into roaster, controls 500 DEG C of temperature, calcination 6 hours.
The solid matter obtained after calcination is added in 45% nitric acid, solid-liquid weight ratio is 1：7, the mistake after boiling 4 hours at 60 DEG C
Filter, rinse filter residue, merging filtrate and flushing liquor.Amalgamation liquid is adjusted near pH to 6.5 with saturated sodium bicarbonate solution, progressively
Saturated aqueous common salt is added, untill a large amount of solids largely separate out, suction filtration obtains solid palladium salt.Solid palladium salt is added into deionization
In water, solid-liquid weight ratio is 1：1, hydrazine hydrate solution is added dropwise while stirring at 70 DEG C, no longer display is obvious in thing to be mixed
During yellow, mixture is filtered, is dried to obtain 13.5g black powder palladium sponges, the rate of recovery 99.1%.
Embodiment 2
1000g is given up palladium solid mixture, wherein 15g containing palladium, is put into roaster, controls 650 DEG C of temperature, calcination 4 hours.
The solid matter obtained after calcination is added in 55% nitric acid, solid-liquid weight ratio is 1：7, the mistake after boiling 4 hours at 80 DEG C
Filter, rinse filter residue, merging filtrate and flushing liquor.Amalgamation liquid is adjusted near pH to 6.5 with saturated potassium hydrogen carbonate solution, progressively
Saturated aqueous common salt is added, untill a large amount of solids largely separate out, suction filtration obtains solid palladium salt.Solid palladium salt is added into deionization
In water, solid-liquid weight ratio is 1：1, hydrazine hydrate solution is added dropwise while stirring at 70 DEG C, no longer display is obvious in thing to be mixed
During yellow, mixture is filtered, is dried to obtain 13.8g black powder palladium sponges, the rate of recovery 99.2%.
Embodiment 3
1000g is given up palladium solid mixture, wherein 15g containing palladium, is put into roaster, controls 900 DEG C of temperature, calcination 3 hours.
The solid matter obtained after calcination is added in 65% nitric acid, solid-liquid weight ratio is 1：8, the mistake after boiling 6 hours at 90 DEG C
Filter, rinse filter residue, merging filtrate and flushing liquor.Amalgamation liquid is adjusted near pH to 6.5 with saturated sodium carbonate solution, progressively added
Enter saturated aqueous common salt, untill a large amount of solids largely separate out, suction filtration obtains solid palladium salt.Solid palladium salt is added into deionized water
In, solid-liquid weight ratio is 1：1, hydrazine hydrate solution is added dropwise while stirring at 70 DEG C, no longer display is obvious yellow in thing to be mixed
During color, mixture is filtered, is dried to obtain 13.2g black powder palladium sponges, the rate of recovery 99.9%.
Embodiment 4
1000g is given up palladium solid mixture, wherein 15g containing palladium, is put into roaster, controls 900 DEG C of temperature, calcination 3 hours.
The solid matter obtained after calcination is added in 55% nitric acid, solid-liquid weight ratio is 1：8, the mistake after boiling 4 hours at 80 DEG C
Filter, rinse filter residue, merging filtrate and flushing liquor.Amalgamation liquid is adjusted near pH to 6.5 with unsaturated carbonate potassium solution, progressively added
Enter saturated aqueous common salt, untill a large amount of solids largely separate out, suction filtration obtains solid palladium salt.Solid palladium salt is added into deionized water
In, solid-liquid weight ratio is 1：1, hydrazine hydrate solution is added dropwise while stirring at 70 DEG C, no longer display is obvious yellow in thing to be mixed
During color, mixture is filtered, is dried to obtain 13.2g black powder palladium sponges, the rate of recovery 99.9%.
Claims (6)
1. a kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste, its characterization step：
Step 1: calcination carbon removal：
By the discarded object containing palladium at 500-900 DEG C calcination 3-6 hours；
Step 2: acid is molten to remove solid impurity：
The solid matter obtained after toward calcination is added in the nitric acid that mass concentration is 45-65%, solid-to-liquid ratio 1：7-9, at 60-90 DEG C
Filtered after lower boiling 3-6 hours, rinse filter residue, merging filtrate and flushing liquor；
Step 3: regulation pH：
Room temperature is controlled, with inorganic salt solution by near the amalgamation liquid regulation pH to 6.5 in step 2, is gradually added into saturated aqueous common salt,
Untill solid separates out, suction filtration obtains solid palladium salt；
Step 4: the reduction of palladium salt：
The solid palladium salt obtained in step 3 is added in deionized water, solid-to-liquid ratio 1：1, hydrazine hydrate solution is added dropwise at 70 DEG C,
When yellow is no longer shown in thing to be mixed, mixture is filtered, is dried to obtain black powder palladium sponge.
2. method according to claim 1, it is characterised in that：Chemical solids discarded object is useless palladium charcoal and useless palladium dydroxide.
3. method according to claim 1, it is characterised in that：Dead palladium catalyst calcination temperature is 500-900 DEG C.
4. method according to claim 1, it is characterised in that：It is nitric acid that acid, which boils acid used, and its mass concentration is 45% to 65%,
It is 60-90 DEG C that acid, which boils temperature used, and it is 3-6 hours that acid, which boils the time used,.
5. method according to claim 1, it is characterised in that：Adjusting pH to 6.5, nearby inorganic salts used are sodium acid carbonate,
Saleratus, sodium carbonate, one kind in potassium carbonate, adjusting needs to control room temperature during pH, and saline solution used is saturated common salt
Water.
6. method according to claim 1, it is characterised in that：Institute's amount of water is one times of palladium salt quality, added hydrazine hydrate
Weight is 6-10 times of palladium salt.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610615841.2A CN107663583A (en) | 2016-07-30 | 2016-07-30 | A kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610615841.2A CN107663583A (en) | 2016-07-30 | 2016-07-30 | A kind of method that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste |
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| CN107663583A true CN107663583A (en) | 2018-02-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110735041A (en) * | 2019-08-28 | 2020-01-31 | 广西银亿高新技术研发有限公司 | process method for leaching insoluble metal waste by cyclic catalytic oxidation acid leaching |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102172776A (en) * | 2011-01-25 | 2011-09-07 | 西安凯立化工有限公司 | Method for preparing metal palladium powder |
| CN103394347A (en) * | 2013-07-23 | 2013-11-20 | 河海大学 | Preparation method of high-activity palladium-carbon catalyst |
| CN103555957A (en) * | 2013-11-20 | 2014-02-05 | 浙江省冶金研究院有限公司 | Method for recovering high-purity metal palladium from organic waste palladium contained catalyst |
-
2016
- 2016-07-30 CN CN201610615841.2A patent/CN107663583A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102172776A (en) * | 2011-01-25 | 2011-09-07 | 西安凯立化工有限公司 | Method for preparing metal palladium powder |
| CN103394347A (en) * | 2013-07-23 | 2013-11-20 | 河海大学 | Preparation method of high-activity palladium-carbon catalyst |
| CN103555957A (en) * | 2013-11-20 | 2014-02-05 | 浙江省冶金研究院有限公司 | Method for recovering high-purity metal palladium from organic waste palladium contained catalyst |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110735041A (en) * | 2019-08-28 | 2020-01-31 | 广西银亿高新技术研发有限公司 | process method for leaching insoluble metal waste by cyclic catalytic oxidation acid leaching |
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