CN107663591A - A kind of method that Metal Palladium is reclaimed from dead palladium catalyst - Google Patents
A kind of method that Metal Palladium is reclaimed from dead palladium catalyst Download PDFInfo
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- CN107663591A CN107663591A CN201610617022.1A CN201610617022A CN107663591A CN 107663591 A CN107663591 A CN 107663591A CN 201610617022 A CN201610617022 A CN 201610617022A CN 107663591 A CN107663591 A CN 107663591A
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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
- 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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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
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Abstract
The invention provides a kind of method that precious metal palladium is reclaimed from dead palladium catalyst.This method includes acid treatment and reducing agent is handled.This method is simple to operation, is adapted to general factory's Recover palladium, is recycled, both reduce production cost, reduce environmental pollution again.Palladium recovery rate is more than 99%.
Description
Technical field
The present invention is to be related to the rear place of chemical field technique on a kind of method that Metal Palladium is reclaimed from dead palladium catalyst
Reason.
Background technology
Palladium charcoal is a kind of important catalyst, and it is widely used in the reduction of nitro, the reduction of carbon-carbon double bond, benzyl
Slough, the hydrogenolysis of carbonyl, the disengaging of fragrant halogen, in the preparation of hydrogenated rosin etc. some chemical reactions.Palladium dydroxide is also made
For a kind of presence of form of palladium catalyst, its catalytic activity is better than palladium charcoal, the reaction that can typically use palladium charcoal to be catalyzed, can also use
Palladium dydroxide.Some reactions change palladium dydroxide into regard to that can be smoothed out because the catalytic activity of palladium charcoal is inadequate.Some fine chemistry industries
Company, medicine intermediate company, both palladium catalysts are generally provided with, often two kinds of palladium catalysts after use are concentrated
To handle.Sometimes it can also separate and handle.The method for the Recover palladium from useless palladium charcoal is reported many at present, but is urged on useless palladium
The research of agent recovery Metal Palladium is not a lot.
The content of the invention
The present invention relates to it is a kind of from dead palladium catalyst reclaim Metal Palladium method, have it is simple to operate, raw material is inexpensively easy
The features such as obtaining.
The technical solution adopted for the present invention to solve the technical problems comprises the following steps：
Step 1: remove solid impurity：
The solid matter obtained after calcination is added in acid, solid-to-liquid ratio 1：7, filtered after 2-4 hours are stirred at room temperature,
Rinse filter residue, merging filtrate and flushing liquor；
Step 2: remove organic matter：
The amalgamation liquid obtained in step 1 is washed 3 to 5 times with dichloromethane；
Step 3: regulation pH：
Room temperature is controlled, the amalgamation liquid after being washed in step 2 is adjusted into pH to 6.5 with inorganic salts, is gradually added into saturated common salt
Water, untill no 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, reduction is added dropwise at 60 DEG C
Agent, when no longer showing obvious yellow 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 dead palladium catalyst, the dead palladium catalyst is palladium dydroxide.
Further, it is a kind of from dead palladium catalyst reclaim Metal Palladium method, acid used can be hydrochloric acid, sulfuric acid,
Nitric acid, preferably hydrochloric acid；Acid molten mixing time 2-4 hours, preferably 3 hours.
Further, a kind of method that Metal Palladium is reclaimed from dead palladium catalyst, adjust in step 3 inorganic used in pH to 6.5
Salt is sodium acid carbonate, saleratus, sodium carbonate, one kind in potassium carbonate, preferably sodium acid carbonate；Saline solution used is saturated common salt
Water.
Further, a kind of method that Metal Palladium is reclaimed from dead palladium catalyst, described reducing agent can be hydroboration
One or more in sodium, potassium borohydride, formic acid, formaldehyde, hydrazine hydrate, preferably hydrazine hydrate；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 dead palladium catalyst, raw material is cheap and easy to get, simple to operate,
The rate of recovery is high.
Embodiment
The scheme that Metal Palladium is reclaimed from useless palladium hybrid solid chemical waste of the present invention is carried out further below
Description, allows those skilled in the art to be better understood by and utilize the present invention.
Embodiment 1
500g is given up palladium dydroxide solid waste, wherein 7.5g containing palladium, is added in 36% hydrochloric acid, solid-liquid weight ratio is
1：7, filtered after being stirred at room temperature 3 hours, rinse filter residue, merging filtrate and flushing liquor.Washed with dichloromethane and merged three times
Liquid is simultaneously at room temperature being adjusted amalgamation liquid near pH to 6.5 with saturated sodium bicarbonate solution, is gradually added saturated aqueous common salt, directly
Untill no solid separates out, suction filtration obtains solid palladium salt.Solid palladium salt is added in deionized water, solid-liquid weight ratio is 1：1,
Hydrazine hydrate solution is added dropwise while stirring at 60 DEG C, when no longer showing obvious yellow in thing to be mixed, mixture is filtered, does
It is dry to obtain 7.4g black powder palladium sponges, the rate of recovery 99.1%.
Embodiment 2
500g is given up palladium dydroxide solid waste, wherein 7.5g containing palladium, is added in 45% nitric acid, solid-liquid weight ratio is
1：7, filtered after being stirred at room temperature 2 hours, rinse filter residue, merging filtrate and flushing liquor.Washed with dichloromethane and merged three times
Liquid is simultaneously using saturated potassium hydrogen carbonate solution to adjust amalgamation liquid near pH to 6.5 at room temperature, is gradually added saturated aqueous common salt, directly
Untill no solid separates out, suction filtration obtains solid palladium salt.Solid palladium salt is added in deionized water, solid-liquid weight ratio is 1：1,
Formic acid is added dropwise while stirring at 60 DEG C, when no longer showing obvious yellow in thing to be mixed, mixture is filtered, is dried to obtain
7.2g black powder palladium sponges, the rate of recovery 99.0%.
Embodiment 3
500g is given up palladium dydroxide solid waste, wherein 7.5g containing palladium, is added in 40% sulfuric acid, solid-liquid weight ratio is
1：7, filtered after being stirred at room temperature 4 hours, rinse filter residue, merging filtrate and flushing liquor.Washed with dichloromethane and merged three times
Liquid is simultaneously at room temperature being adjusted amalgamation liquid near pH to 6.5 with saturated sodium carbonate solution, is gradually added saturated aqueous common salt, until
Untill not having solid precipitation, suction filtration obtains solid palladium salt.Solid palladium salt is added in deionized water, solid-liquid weight ratio is 1：1,
Solution of potassium borohydride is added dropwise at 60 DEG C while stirring, when no longer showing obvious yellow in thing to be mixed, mixture is filtered, does
It is dry to obtain 6.8g black powder palladium sponges, the rate of recovery 99.6%.
Embodiment 4
500g is given up palladium dydroxide solid waste, wherein 7.5g containing palladium, is added in 40% sulfuric acid, solid-liquid weight ratio is
1：7, filtered after being stirred at room temperature 3 hours, rinse filter residue, merging filtrate and flushing liquor.Washed with dichloromethane and merged three times
Liquid is simultaneously at room temperature being adjusted amalgamation liquid near pH to 6.5 with solution of potassium carbonate, saturated aqueous common salt is gradually added, until not having
Untill solid separates out, suction filtration obtains solid palladium salt.Solid palladium salt is added in deionized water, solid-liquid weight ratio is 1：1, at 60 DEG C
Under formalin is added dropwise while stirring, when no longer showing obvious yellow in thing to be mixed, mixture is filtered, is dried to obtain
6.8g black powder palladium sponges, the rate of recovery 99.5%.
Claims (5)
1. a kind of method that Metal Palladium is reclaimed from dead palladium catalyst, its characterization step：
Step 1: remove solid impurity：
The solid matter obtained after calcination is added in acid, solid-to-liquid ratio 1：7, filter, rinse after 2-4 hours are stirred at room temperature
Filter residue, merging filtrate and flushing liquor；
Step 2: remove organic matter：
The amalgamation liquid obtained in step 1 is washed 3 to 5 times with dichloromethane；
Step 3: regulation pH：
Room temperature is controlled, the amalgamation liquid after being washed in step 2 is adjusted into pH to 6.5 with inorganic salts, is gradually added into saturated aqueous common salt,
Untill no 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, reducing agent is added dropwise at 60 DEG C, treats
When yellow is no longer shown in mixture, mixture is filtered, is dried to obtain black powder palladium sponge.
2. method according to claim 1, it is characterised in that：Handled discarded palladium catalyst is palladium dydroxide.
3. method according to claim 1, it is characterised in that：Acid used can be hydrochloric acid, sulfuric acid, nitric acid in step 1,
It is preferred that hydrochloric acid；Acid molten mixing time 2-4 hours.
4. method according to claim 1, it is characterised in that：It is sodium acid carbonate that inorganic salts used in pH to 6.5 are adjusted in step 3,
Saleratus, sodium carbonate, one kind in potassium carbonate, preferably sodium acid carbonate, the saline solution are saturated aqueous common salt.
5. method according to claim 1, it is characterised in that：Reducing agent described in step 4 can be sodium borohydride, boron
One or more in hydrofining, formic acid, formaldehyde, hydrazine hydrate；Institute's amount of water is one times of palladium salt quality, added hydrazine hydrate
Weight is 6-10 times of palladium salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610617022.1A CN107663591A (en) | 2016-07-30 | 2016-07-30 | A kind of method that Metal Palladium is reclaimed from dead palladium catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610617022.1A CN107663591A (en) | 2016-07-30 | 2016-07-30 | A kind of method that Metal Palladium is reclaimed from dead palladium catalyst |
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| CN107663591A true CN107663591A (en) | 2018-02-06 |
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| CN201610617022.1A Pending CN107663591A (en) | 2016-07-30 | 2016-07-30 | A kind of method that Metal Palladium is reclaimed from dead palladium catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114107663A (en) * | 2021-10-12 | 2022-03-01 | 安徽元琛环保科技股份有限公司 | Method for extracting noble metal from waste noble metal catalyst |
-
2016
- 2016-07-30 CN CN201610617022.1A patent/CN107663591A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114107663A (en) * | 2021-10-12 | 2022-03-01 | 安徽元琛环保科技股份有限公司 | Method for extracting noble metal from waste noble metal catalyst |
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Application publication date: 20180206 |