CN108707751A - A kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid - Google Patents
A kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid Download PDFInfo
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- CN108707751A CN108707751A CN201810634395.9A CN201810634395A CN108707751A CN 108707751 A CN108707751 A CN 108707751A CN 201810634395 A CN201810634395 A CN 201810634395A CN 108707751 A CN108707751 A CN 108707751A
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- desiliconization liquid
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- desiliconization
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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
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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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- Environmental & Geological Engineering (AREA)
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The present invention relates to a kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid, include the following steps：1）Desiliconization liquid is fitted into reaction kettle, is then heated to 50~80 DEG C；2）Liquid reducing agent is added, is 0.001~0.01 by the volume ratio of liquid reducing agent and desiliconization liquid：1；3）0.5~2h is kept the temperature at 50~80 DEG C；4）Desiliconization liquid is heated to 60~90 DEG C：5）Solid state reduction agent is added, the addition of solid state reduction agent is that 10~50g is added in every liter of desiliconization liquid；6) 0.5~5h is kept the temperature at 60~90 DEG C；7) flocculant is added, is 0.0001~0.003 by the volume ratio of flocculant and desiliconization liquid：1；8）Desiliconization liquid filters after settling 3~10h.This method solves the scattering problem of platinum group metal in desiliconization liquid after primary reduction, can restore the platinum group metal in desiliconization liquid completely, and the quantity of slag is few, easy to operate.
Description
Technical field
The invention belongs to noble metal recovery technology fields, relate in particular to platinum group metal, be one kind in high alkalinity desiliconization
The restoring method of low concentration platinum group metal in liquid.
Background technology
Due to the uniqueness of platinum group metal performance and the scarcity of resource, " strategy storage is classified as by many developed countries of the world
Standby metal ", in development for hi-tech industry, is known as " the first high-technology metal ".Platinum group metal also there is excellent catalysis to live
Property, it is widely used in each industrial circle, is referred to as " king of catalysis ", " modern industry vitamin ".
And catalyst is mainly made of carrier and active material two parts, presently used carrier material is mostly aluminium oxide
Carrier, silica-gel carrier etc., main active substances are Pt, Pd and Rh.For the catalyst containing silica-gel carrier after dissolving liquid making shape
At the insoluble slag of high silicon content, to make the noble metal in insoluble slag further be enriched with, after being handled using alkali soluble desiliconization, in desiliconization liquid
In the platinum group metal (platinum, palladium and rhodium) containing low concentration.This desiliconization liquid has high alkalinity（PH > 10）, platinum group metal concentration is low contains
Platinum, palladium, rhodium（Platinum 0.002-0.005g/L, palladium 0.0035-0.01g/L, rhodium 0.0014-0.004g/L）, the features such as volume is big.
It is general in the prior art that this desiliconization liquid is handled using reduction method, even with strong reductant（Such as hydrazine hydrate）Also
Original, effect unobvious have tiny suspension colloid particle that cannot form precipitation, and noble metal cannot be reduced completely in desiliconization liquid.
It needs repeatedly to restore, causes reagent waste, increase processing cost, increase discharge pressure.
Patent CN201310318480.1《Reduction precipitation method recycles platinum from containing low concentration platinum-group noble metals acid solution
The technique of palladium》Disclose a kind of method recycling platinum palladium from noble metal acid feed liquid using reduction precipitation method.With sodium formate and
Sodium borohydride reacts platinum precipitation palladium with platiniferous palladium feed liquid as precipitate reduction agent, and the method is suitable for acid solution, it is impossible to be used in
Alkaline solution.Patent CN200710009132.0 is disclosed《Metal Palladium and palladium bichloride are recycled from waste loading palladium hydrogenation catalyst
Method》, reduction of this method suitable for high concentration palladium salt.Patent CN200610046634.6 is disclosed《One kind is from containing your gold
Belong to the method that noble metal is recycled in dead catalyst》, reduction of this method suitable for high concentration platinum salt.
Urgently propose a kind of reduction easy to operate, low concentration platinum group metal in the preferable high alkalinity desiliconization liquid of recovering effect
Method, to realize the technical solution for recycling platinum group metal in alkaline desiliconization liquor.
Invention content
The present invention provides a kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid.For containing silica-gel carrier
Catalyst the insoluble slag of high silicon content is formed after dissolving liquid making, to make the noble metal in insoluble slag further be enriched with, use
After alkali soluble desiliconization processing, the platinum group metal (platinum, palladium and rhodium) in desiliconization liquid containing low concentration.It solves general in the prior art
This desiliconization liquid is handled using reduction method, even with strong reductant（Such as hydrazine hydrate）Reduction, effect unobvious have tiny hang
Floating colloidal solid cannot form precipitation, and noble metal cannot be reduced completely in desiliconization liquid.It needs repeatedly to restore, causes reagent unrestrained
The problems such as taking, increase processing cost, increasing discharge pressure.
Specific technical solution is：A kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid, including it is as follows
Step：
1）Desiliconization liquid is fitted into reaction kettle, is then heated to 50~80 DEG C；
2）Liquid reducing agent is added, is 0.001~0.01 by the volume ratio of liquid reducing agent and desiliconization liquid：1；
3）0.5~2h is kept the temperature at 50~80 DEG C；
4）Desiliconization liquid is heated to 60~90 DEG C：
5）Solid state reduction agent is added, the addition of solid state reduction agent is that 10~50g is added in every liter of desiliconization liquid；
6) 0.5~5h is kept the temperature at 60~90 DEG C；
7) flocculant is added, is 0.0001~0.003 by the volume ratio of flocculant and desiliconization liquid：1；
8）Desiliconization liquid filters after settling 3~10h.
Further, the of the present invention 1st）In step, the desiliconization liquid is in alkalinity.
Further, the of the present invention 1st）In step, the reaction kettle is steam-heated plastics reaction kettle either titanium
The reaction kettle of material；The heating temperature is 50~80 DEG C, preferably 55~65 DEG C.
Further, the of the present invention 2nd）In step, the liquid reducing agent is 80% technical grade hydrazine hydrate, 40% technical grade
Hydrazine hydrate or formic acid, preferably 80% technical grade hydrazine hydrate, addition are to be by the volume ratio of liquid reducing agent and desiliconization liquid
0.001~0.01：1, preferably 0.003~0.006:1.
Further, the of the present invention 3rd）In step, the holding temperature is 50~80 DEG C, preferably 55~65 DEG C；
Soaking time is 0.5 ~ 2h, preferably 1~1.5h.
Further, the of the present invention 4th）In step, the heating temperature is 60~90 DEG C, preferably 70~80 DEG C.
Further, the of the present invention 5th）In step, the solid state reduction agent be technical grade sodium formate or glucose, preferably
Be technical grade sodium formate, addition is that 10~50g, preferably 15~40g are added in every liter of desiliconization liquid.
Further, the of the present invention 6th）In step, the holding temperature is 60~90 DEG C, preferably 70~80 DEG C；
Soaking time is 0.5~5h, preferably 1~4h.
Further, the of the present invention 7th）In step, the flocculant is calcium polyacrylate (CPA), acrylic acid or polyacrylamide
Amine, preferably liquid macroimolecule flocculant, preferably cation, ion degree 5~80, molecular weight 500~12,000,000 poly- third
Acrylamide, a concentration of 0.2~0.4%；The addition of the flocculant by the volume ratio of flocculant and desiliconization liquid be 0.0001~
0.003：1, preferably 0.0002~0.001:1.
Further, the of the present invention 8th）In step, the sedimentation time is 2~10h, preferably 3~8h.
Further, the of the present invention 8th）After step, gained filtrate sample presentation detects bullion content.
The present invention does not do particular determination to the acquisition modes of used desiliconization liquid, is obtained using method known in the art
, it is obtained as method described in CN105621429A may be used.
Beneficial effects of the present invention：The restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid, this method are provided
The scattering problem that platinum group metal in desiliconization liquid is solved after once restoring, can restore the platinum group metal in desiliconization liquid, make completely
Platinum group metal content in desiliconization liquid after reduction is less than 0.0005g/L.And the quantity of slag is few, it is easy to operate.
Specific implementation mode
In order to make technical problem solved by the invention, technical solution be more clearly understood, by the following examples, to this
Invention is further described.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used to
Limit the present invention.Keep the understanding to the disclosure more thorough complete on the contrary, purpose of providing these embodiments is
Face.
It is analyzed using inductively coupled plasma atomic emission spectrometry (ICP-AES) in following embodiment and comparative example
Platinum, palladium, rhodium content in solution.
Embodiment 1：
Desiliconization liquid used by the embodiment is pressed 1 the method for embodiment in CN105621429A and is made.
PH is fitted into more than 7 1500L desiliconization liquids in steam-heated plastics reaction, and is heated to 60 DEG C, is added at this time
80% technical grade hydrazine hydrate 6L, keeps the temperature 1h at 60 DEG C after adding, be heated to 75 DEG C later, and technical grade sodium formate 30kg is added, adds
3h is kept the temperature after complete at 75 DEG C, flocculant 900ml is then added, stops heating after adding, closing agitating paddle keeps solution naturally cold
But, solution inspection is taken to analyze after settling 6h.Testing result is shown in Table 1.
Table 1
Comparative example 1：
Other conditions are same as Example 1, the difference is that only having added 80% technical grade hydrazine hydrate, do not add sodium formate and flocculation
Agent.Laboratory test results are shown in Table 2.
Table 2
Embodiment 2：
Desiliconization liquid used by the embodiment is pressed 1 the method for embodiment in CN105621429 A and is made.
PH is fitted into more than 7 2000L desiliconization liquids in steam-heated plastics reaction, and is heated to 65 DEG C, is added at this time
80% technical grade hydrazine hydrate 10L, keeps the temperature 1.5h at 65 DEG C after adding, be heated to 80 DEG C later, and technical grade sodium formate is added
40kg keeps the temperature 3.5h at 80 DEG C after adding, flocculant 1.5L is then added, and stops heating after adding, and closing agitating paddle makes molten
Liquid natural cooling takes solution inspection to analyze after settling 8h.Testing result is shown in Table 3.
Table 3
Comparative example 2：
Other conditions are same as Example 2, the difference is that the addition of sodium formate and flocculant does not press the ratio row of the present invention
It is added.Laboratory test results are shown in Table 4.
Table 4
Embodiment 3：
Desiliconization liquid used by the embodiment is pressed 1 the method for embodiment in CN105621429 A and is made.
PH is fitted into more than 7 1600L desiliconization liquids in steam-heated plastics reaction, and is heated to 65 DEG C, is added at this time
80% technical grade hydrazine hydrate 8L, keeps the temperature 1.5h at 65 DEG C after adding, be heated to 80 DEG C later, and technical grade sodium formate 45kg is added,
3h is kept the temperature after adding at 80 DEG C, flocculant 1.2L is then added, stops heating after adding, closing agitating paddle keeps solution naturally cold
But, solution inspection is taken to analyze after settling 8h.Testing result is shown in Table 5.
Table 5
Comparative example 3：
Other conditions are same as Example 3, the difference is that the four, the six step heating temperatures are not within the scope of the present invention.
Laboratory test results are shown in Table 6.
Table 6
The present invention is described in detail above by specific and preferred embodiment, but it will be understood by those skilled in the art that
The invention is not limited in embodiment described above, all within the spirits and principles of the present invention, made by any modification, equivalent
Replace etc., it should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid, it is characterised in that：Include the following steps：
1）Desiliconization liquid is fitted into reaction kettle, is then heated to 50~80 DEG C；
2）Liquid reducing agent is added, is 0.001~0.01 by the volume ratio of liquid reducing agent and desiliconization liquid：1；
3）0.5~2h is kept the temperature at 50~80 DEG C；
4）Desiliconization liquid is heated to 60~90 DEG C：
5）Solid state reduction agent is added, the addition of solid state reduction agent is that 10~50g is added in every liter of desiliconization liquid；
6) 0.5~5h is kept the temperature at 60~90 DEG C；
7) flocculant is added, is 0.0001~0.003 by the volume ratio of flocculant and desiliconization liquid：1；
8）Desiliconization liquid filters after settling 3~10h.
2. a kind of restoring method of low concentration platinum group metal in high alkalinity desiliconization liquid according to claim 1, feature
It is：The described 1st）In step, the desiliconization liquid is in alkalinity.
3. a kind of restoring method of low concentration platinum group metal in high alkalinity desiliconization liquid according to claim 1, feature
It is：The described 2nd）In step, the liquid reducing agent is 80% technical grade hydrazine hydrate, 40% technical grade hydrazine hydrate or formic acid.
4. a kind of restoring method of low concentration platinum group metal in high alkalinity desiliconization liquid according to claim 1, feature
It is：The described 5th）In step, the solid state reduction agent is solid industrial grade sodium formate or glucose.
5. a kind of restoring method of low concentration platinum group metal in high alkalinity desiliconization liquid according to claim 1, feature
It is：The described 7th）In step, the flocculant is calcium polyacrylate (CPA), acrylic acid or the polyacrylamide of solution-type.
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| CN201810634395.9A CN108707751A (en) | 2018-06-20 | 2018-06-20 | A kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid |
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| CN201810634395.9A CN108707751A (en) | 2018-06-20 | 2018-06-20 | A kind of restoring method of the low concentration platinum group metal in high alkalinity desiliconization liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021212936A1 (en) | 2020-04-23 | 2021-10-28 | 贺利氏贵金属技术(中国)有限公司 | Method for recovering precious metal from precious metal-containing waste catalyst |
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| CN105039717A (en) * | 2015-09-10 | 2015-11-11 | 苏州联科纳米净化科技有限公司 | Method for recycling palladium from alkaline palladium activation section waste water |
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2018
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Patent Citations (4)
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| CN102443707A (en) * | 2011-11-30 | 2012-05-09 | 徐州浩通新材料科技股份有限公司 | Method for recycling platinum from organic alcohol waste liquor |
| CN103194606A (en) * | 2013-03-28 | 2013-07-10 | 贵研资源（易门）有限公司 | Method for concentrating platinum group metals from alumina-based waste catalyst |
| CN104726899A (en) * | 2014-12-30 | 2015-06-24 | 永兴贵研资源有限公司 | Method for recycling silver and platinum from platinum-containing silver iodide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021212936A1 (en) | 2020-04-23 | 2021-10-28 | 贺利氏贵金属技术(中国)有限公司 | Method for recovering precious metal from precious metal-containing waste catalyst |
| EP4141134A4 (en) * | 2020-04-23 | 2024-05-22 | Heraeus Precious Metal Tech China Co Ltd | Method for recovering precious metal from precious metal-containing waste catalyst |
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