CN107267762A - A kind of method of Palladium recovery in palladium activation waste water - Google Patents
A kind of method of Palladium recovery in palladium activation waste water Download PDFInfo
- Publication number
- CN107267762A CN107267762A CN201710528263.3A CN201710528263A CN107267762A CN 107267762 A CN107267762 A CN 107267762A CN 201710528263 A CN201710528263 A CN 201710528263A CN 107267762 A CN107267762 A CN 107267762A
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- Prior art keywords
- palladium
- waste water
- activated carbon
- present
- recovery
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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
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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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
Abstract
The method that the present invention provides Palladium recovery in a kind of palladium activation waste water.The method of Palladium recovery comprises the following steps in the palladium activation waste water that the present invention is provided：Palladium activation waste water is flowed through into Palladium recovery system and carries out adsorption treatment, the Palladium recovery system includes activated carbon；Activated carbon after the adsorption treatment is burned, Metal Palladium is obtained.The present invention compares the absorption pore-size distribution of wide scope using activated carbon, and the palladium and the palladium of free state in micelle are fully adsorbed, the influence of excess Sn elements in activating solution is avoided using the method for physical absorption.Test result indicates that, the method that provides of the present invention effectively can activate colloid palladium and free palladium in waste water by Recover palladium, and the yield of palladium can reach more than 90%.
Description
Technical field
The present invention relates to metal material utilization technology field, more particularly to a kind of palladium activates the side of Palladium recovery in waste water
Method.
Background technology
Colloidal pd activation solution is electroplating industry, especially most widely used catalysis in plastic cement plating and PCB aperture metallization
Agent.Either plastic cement plating or PCB aperture metallization are required for producing active centre first on non electrically conductive material surface, adopt
Conducting film is formed with chemical plating or displacement plating, the overall process then thickeied with routinely electroplating.Before this, it is necessary to plastics
Matrix carries out surface preparation, and committed step is activation.Pd/Sn colloid catalysts are most widely used glue in activation process
Body palladium, it is by PdCl2And SnCl2Reaction is prepared from an acidic solution, and glue core is palladium, and outer layer is the divalence and tetravalence of aquation
Tin ion, excessive Sn2+Stabilization to the catalytic liquid plays a crucial role.
In palladium activation production process, workpiece is submerged initially in the activating solution in palladium activated bath, immersion a period of time, proposes workpiece
Hovering a period of time, then successively immersion 1,2,3 road wash waters in, wash water use overflow pattern, by 3 groove moisturizings, overflow to 2 grooves, then
By 2 groove overflows to 1 groove, emitted by 1 groove.Palladium in activating solution is general in tens to hundreds of ppm, after a period of time
Impurity is constantly accumulated, and content is raised, it is necessary to the activating solution more renewed；The palladium also containing the several ppm of zero point in overflow water is cleaned, often
Its several tons to tens tons discharge, all along with the loss of palladium.
Palladium is noble metal, is scarce resource, with the Palladium recovery difficulty pole in recovery value, but activating solution and rinse water
Greatly, its main cause is that colloid is different from SOLUTION PROPERTIES, and palladium is difficult to be captured as the glue core of micelle.Colloid of the prior art
Palladium recovery method is all, by the broken glue method of heating or the broken glue method of oxidation, palladium ion to be obtained while colloid is removed, then through also
Original precipitation obtains Metal Palladium, but is due to that Sn ions are present in excess in activating solution, is tens concentration for arriving hundred times palladium, in reduction
During can influence the recovery and separation of palladium ion；Also, it is extremely low to clean palladium concentration in overflow water, sometimes less than 1ppm, water
Huge, several tons to tens tons of the daily treating capacity of every line is measured, the effect of precipitate reduction is influenceed.These features have all had a strong impact on palladium
The recovery of palladium in waste water is activated, thus major part uses the factory of palladium activating solution to be all directly discharged to palladium activating solution and rinse water
Waste water processing station, therefore there is huge waste.
The content of the invention
It is an object of the invention to provide the method for Palladium recovery in a kind of palladium activation waste water.The palladium activation that the present invention is provided is useless
The method of Palladium recovery is without broken glue processing in water, and the high income of palladium, purity is high.
The invention provides the method for Palladium recovery in a kind of palladium activation waste water, comprise the following steps：
(1) palladium activation waste water is flowed through into Palladium recovery system and carries out adsorption treatment, the Palladium recovery system includes activated carbon；
(2) activated carbon after the adsorption treatment is burned, obtains Metal Palladium.
It is preferred that, the Palladium recovery system includes being filled with activated carbon in adsorption barrel, the adsorption barrel.
It is preferred that, the specific surface area of the activated carbon is 500m2/ more than g.
It is preferred that, the quantity of the adsorption barrel is 1~4.
It is preferred that, the volume of the adsorption barrel is 20~100L.
It is preferred that, the flow velocity of the palladium activation waste water is 10~800L/h.
It is preferred that, the palladium activation waste water includes palladium activating solution and/or rinse water.
It is preferred that, the palladium in the palladium activation waste water includes colloid palladium and/or free palladium.
It is preferred that, the mass concentration of palladium is 10~800ppm in the palladium activating solution.
It is preferred that, the mass concentration of palladium is 0.1~5ppm in the rinse water.
The invention provides the method for Palladium recovery in a kind of palladium activation waste water, comprise the following steps：Palladium is activated into waste water stream
Adsorption treatment is carried out through Palladium recovery system, the Palladium recovery system includes activated carbon；By the activated carbon after the adsorption treatment
Burned, obtain Metal Palladium.The present invention compares the absorption pore-size distribution of wide scope using activated carbon, to the palladium in micelle and trip
The palladium of amorph is fully adsorbed, and the influence of excess Sn elements in activating solution is avoided using the method for physical absorption.Experiment knot
Fruit shows, the method that provides of the present invention effectively can activate colloid palladium and free palladium in waste water by Recover palladium, and the yield of palladium can be with
Reach more than 90%.
Brief description of the drawings
Fig. 1 is palladium activation and Palladium recovery system structure diagram in the embodiment of the present invention 1.
Embodiment
The invention provides the method for Palladium recovery in a kind of palladium activation waste water, comprise the following steps：
(1) palladium activation waste water is flowed through into Palladium recovery system and carries out adsorption treatment, the Palladium recovery system includes activated carbon；
(2) activated carbon after the adsorption treatment is burned, obtains Metal Palladium.
Palladium activation waste water is flowed through Palladium recovery system and carries out adsorption treatment by the present invention, and the Palladium recovery system includes activity
Charcoal.In the present invention, the activated carbon can fully be inhaled as sorbing material to the free palladium and colloid palladium in waste water
It is attached, and physical absorption is adsorbed as, do not influenceed by other elements in waste water.
In the present invention, the palladium activation waste water preferably includes palladium activating solution and/or rinse water.In the present invention, it is described
Palladium in palladium activation waste water preferably includes colloid palladium and/or free palladium.In the present invention, the quality of palladium is dense in the palladium activating solution
Degree is preferably 10~800ppm, most preferably more preferably 50~500ppm, 100~300ppm.In the present invention, the cleaning
The mass concentration of palladium is preferably 0.1~5ppm in water, more preferably 0.3~3ppm, most preferably 0.5~1ppm.In the present invention
In, the colloid palladium and free palladium that the activated carbon in the Palladium recovery system activates various concentrations in waste water to palladium all have well
Adsorption effect.
The present invention does not have special restriction to the structure of the Palladium recovery system, and waste water can be made to adequately flow through activated carbon i.e.
Can.In the present invention, the Palladium recovery system preferably includes to be filled with activated carbon in adsorption barrel, the adsorption barrel.The present invention is excellent
The specification for activating production according to palladium is selected to select the quantity and volume of adsorption barrel.In the present invention, the quantity of the adsorption barrel is preferred
For 1~4, more preferably 2~3.In the present invention, the volume of the adsorption barrel is preferably 20~100L, and more preferably 30
~80L, most preferably 50~60L.In the present invention, the specific surface area of the activated carbon is preferably 500m2/ more than g, more preferably
For 520~600m2/g.In the present invention, the aperture of the activated carbon is preferably below 150nm, more preferably 10~100nm.
In the present invention, the flow velocity of the palladium activation waste water is preferably 10~800L/h, and more preferably 50~500L/h is most preferably
100~300L/h.In the present invention, the ratio table of the quantity of the flow velocity of the palladium activation waste water and adsorption barrel, volume and activated carbon
Area coordinates, and can further ensure that the palladium in palladium activation waste water is fully adsorbed.
In the present invention, the Palladium recovery system preferably also includes cleaning device and the absorption being communicated in palladium activation system
Temporary storage barrel between bucket.The present invention does not have special restriction to the volume of the temporary storage barrel, is entered according to the specification that palladium activates production
Row adjustment.After the palladium activating solution more swapped out in the activated bath is preferably discharged into and mixed in temporary storage barrel with cleaning fluid by the present invention
Carry out adsorption treatment.
In the present invention, water pump is preferably also included between the temporary storage barrel and adsorption barrel.In the present invention, the water pump energy
Palladium recovery waste water is enough set to flow into adsorption barrel from temporary storage barrel, while controlling the flow velocity of Palladium recovery waste water.
To ensure quality of adsorption, the present invention preferably reaches that the activated carbon more renewed after saturation is inhaled in the activated carbon
It is attached.In the present invention, when palladium concentration is unchanged in waste water before and after the absorption, activated carbon reaches saturation.
After the completion of absorption, the present invention is burned the activated carbon after the adsorption treatment, obtains Metal Palladium.The present invention is right
Charcoal and organic matter can be burnt out, be separated with Metal Palladium without special restriction by the operation of the burning.
The present invention compares the absorption pore-size distribution of wide scope using activated carbon, and the palladium of the palladium in micelle and free state is carried out
Fully absorption, the influence using excess Sn elements in activating solution during reduction precipitation method, palladium are avoided using the method for physical absorption
The rate of recovery is high, and purity is high；And whole adsorption system with activate producing line do not have it is any interact, there is no any shadow for activation process
Ring, modular operation, easy installation and removal, beneficial to popularization.
In order to further illustrate the present invention, Palladium recovery in waste water is activated to the palladium that the present invention is provided with reference to embodiment
Method is described in detail, but they can not be interpreted as into limiting the scope of the present invention.
Embodiment 1:
Company A producing line, activates sump volume 900L, and every three months changes palladium concentration in a palladium activating solution, palladium activating solution
Palladium concentration 0.3ppm in 25ppm, rinse water flooding velocity 400L/h, overflow water.
Palladium activate and Palladium recovery system schematic as shown in figure 1, change after palladium activating solution and the cleaned row of groove 1 of overflow water
Enter the temporary storage barrel in Palladium recovery system, flowed into after adsorption system carries out adsorption treatment and discharged with 400L/h speed through water pump；It is described
Adsorption system includes being filled with specific surface area in the adsorption barrel that two volumes are 25L, adsorption barrel for 520m2/ g activated carbon.
Three months saturations of charcoal absorption in the present embodiment, adsorb palladium about 190g, the yield of palladium is 90%.
Embodiment 2:
B companies producing line, activates sump volume 1800L, and every three months changes palladium concentration in a palladium activating solution, palladium activating solution
Palladium concentration 0.5ppm in 30ppm, rinse water flooding velocity 600L/h, overflow water.
The temporary storage barrel that palladium activating solution and the cleaned groove of overflow water after replacing are discharged into Palladium recovery system, through water pump with
600L/h speed flows into adsorption system and discharged after adsorption treatment；The adsorption system includes the suction that two volumes are 50L
Specific surface area is filled with attached bucket, adsorption barrel for 520m2/ g activated carbon.
One month saturation of charcoal absorption in the present embodiment, adsorbs palladium about 160g, the yield of palladium is 90%.
Embodiment 3:
C companies producing line, activates sump volume 200L, and every three months changes a palladium activating solution, palladium concentration 200ppm, rinse water
Palladium concentration 2.5ppm in flooding velocity 100L/h, overflow water.
The temporary storage barrel that palladium activating solution and the cleaned groove of overflow water after replacing are discharged into Palladium recovery system, through water pump with
100L/h speed flows into adsorption system and discharged after adsorption treatment；The adsorption system includes the suction that two volumes are 50L
Specific surface area is filled with attached bucket, adsorption barrel for 520m2/ g activated carbon.
One month saturation of charcoal absorption in the present embodiment, adsorbs palladium about 150g, the yield of palladium is 90%.
As can be seen from the above embodiments, the method that the present invention is provided can activate the colloid palladium in waste water and dissociate to palladium
Palladium is effectively adsorbed, and whole adsorption system does not influence on activation producing line, modular operation, easy installation and removal, profit
In popularization.
Described above is only the preferred embodiment of the present invention, not makees any formal limitation to the present invention.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. the method for Palladium recovery, comprises the following steps in a kind of palladium activation waste water：
(1) palladium activation waste water is flowed through into Palladium recovery system and carries out adsorption treatment, the Palladium recovery system includes activated carbon；
(2) activated carbon after the adsorption treatment is burned, obtains Metal Palladium.
2. according to the method described in claim 1, it is characterised in that the Palladium recovery system includes adsorption barrel, the adsorption barrel
In be filled with activated carbon.
3. method according to claim 1 or 2, it is characterised in that the specific surface area of the activated carbon is 500m2/ more than g.
4. method according to claim 3, it is characterised in that the quantity of the adsorption barrel is 1~4.
5. method according to claim 4, it is characterised in that the volume of the adsorption barrel is 20~100L.
6. according to the method described in claim 1, it is characterised in that the flow velocity of the palladium activation waste water is 10~800L/h.
7. the method according to claim 1 or 6, it is characterised in that the palladium activation waste water includes palladium activating solution and/or clear
Wash water.
8. method according to claim 7, it is characterised in that the palladium in the palladium activation waste water include colloid palladium and/or
Free palladium.
9. method according to claim 8, it is characterised in that in the palladium activating solution mass concentration of palladium be 10~
800ppm。
10. method according to claim 8, it is characterised in that in the rinse water mass concentration of palladium be 0.1~
5ppm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710528263.3A CN107267762A (en) | 2017-07-01 | 2017-07-01 | A kind of method of Palladium recovery in palladium activation waste water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710528263.3A CN107267762A (en) | 2017-07-01 | 2017-07-01 | A kind of method of Palladium recovery in palladium activation waste water |
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| CN107267762A true CN107267762A (en) | 2017-10-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710528263.3A Pending CN107267762A (en) | 2017-07-01 | 2017-07-01 | A kind of method of Palladium recovery in palladium activation waste water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987877A (en) * | 2017-04-01 | 2017-07-28 | 厦门建霖工业有限公司 | A kind of plastic electroplating colloid Palladium recovery and the system and method for Water circulation |
| JP2020146633A (en) * | 2019-03-14 | 2020-09-17 | 松田産業株式会社 | Method and apparatus for collecting catalyst metal from aqueous solution containing catalyst metal coprecipitated with tin |
| CN112159898A (en) * | 2020-01-17 | 2021-01-01 | 倍永环保科技（上海）有限公司 | Palladium recovery method for printed circuit board factory |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186718A (en) * | 1996-12-30 | 1998-07-08 | 韦士平 | Process for reclaiming waste catalyst with low palladium content |
| CN102808084A (en) * | 2012-08-14 | 2012-12-05 | 云南大学 | Method for enriching platinum and palladium from pressurized cyanating solution |
| CN104685075A (en) * | 2012-06-22 | 2015-06-03 | 可乐丽化学株式会社 | Activated carbon for noble metal adsorption, noble metal adsorption filter, and method for recovering noble metals |
-
2017
- 2017-07-01 CN CN201710528263.3A patent/CN107267762A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186718A (en) * | 1996-12-30 | 1998-07-08 | 韦士平 | Process for reclaiming waste catalyst with low palladium content |
| CN104685075A (en) * | 2012-06-22 | 2015-06-03 | 可乐丽化学株式会社 | Activated carbon for noble metal adsorption, noble metal adsorption filter, and method for recovering noble metals |
| CN102808084A (en) * | 2012-08-14 | 2012-12-05 | 云南大学 | Method for enriching platinum and palladium from pressurized cyanating solution |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987877A (en) * | 2017-04-01 | 2017-07-28 | 厦门建霖工业有限公司 | A kind of plastic electroplating colloid Palladium recovery and the system and method for Water circulation |
| JP2020146633A (en) * | 2019-03-14 | 2020-09-17 | 松田産業株式会社 | Method and apparatus for collecting catalyst metal from aqueous solution containing catalyst metal coprecipitated with tin |
| WO2020183946A1 (en) * | 2019-03-14 | 2020-09-17 | 松田産業株式会社 | Method and device for recovering catalytic metal from aqueous solution including catalytic metal coprecipitated with tin |
| CN112159898A (en) * | 2020-01-17 | 2021-01-01 | 倍永环保科技（上海）有限公司 | Palladium recovery method for printed circuit board factory |
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Application publication date: 20171020 |