CN106636652A - Technique for efficient and environment-friendly recovery of palladium from sliver anode slime parting liquid - Google Patents
Technique for efficient and environment-friendly recovery of palladium from sliver anode slime parting liquid Download PDFInfo
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- CN106636652A CN106636652A CN201611173336.3A CN201611173336A CN106636652A CN 106636652 A CN106636652 A CN 106636652A CN 201611173336 A CN201611173336 A CN 201611173336A CN 106636652 A CN106636652 A CN 106636652A
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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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- 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
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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
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Abstract
The invention provides a technique for efficient and environment-friendly recovery of palladium from sliver anode slime parting liquid. The technique is mainly comprises the following stages of concentration and crystallization of the parting liquid, washing of deposited silver of the parting liquid, oxidation and palladium deposition, impurity-removing purification, palladium reduction, and drying. According to the technique, all adopted equipment are conventional equipment, operation is easy, the cost of adopted agents is low, the pH value of an original solution does not need to be regulated, production efficiency is high, and environmental friendliness is achieved. The obtained palladium is high in purity and good in quality, and the technique is suitable for the production practice of extracting palladium from low-concentration palladium-containing solutions.
Description
Technical field
The present invention relates in a kind of parting liquid from silver anode slime efficient green Recover palladium technique, belong to noble metal wet method smelting
Gold process technical field.
Background technology
Platinum family element content in the earth's crust is rare, and palladium is one kind of platinum group metal, and it has significant physicochemical properties,
It is widely used, there is very important effect in the fields such as chemical industry, national defence scientific research.The synthetical recovery of Domestic Palladium is adopted from two mostly
Extract in secondary resource, but secondary resource species is more, and grade is greatly different and impurity is different, causes the generation rate of recovery low, process contamination
Serious the problems such as.
The main component of silver electrolysis anode slime is silver-colored, golden and a small amount of platinum palladium metal, is leached silver and palladium using nitric acid
Parting liquid is obtained, its main component is silver nitrate.It is common except Ag+Agent is hydrochloric acid, if directly using the heavy silver of hydrochloric acid, hydrochloric acid consumption
Greatly, the volatile operating condition of hydrochloric acid is poor, and the substantial amounts of silver nitride precipitation of generation need to return to silver-colored pyrometallurgical smelting.Palladium in parting liquid
Levels it is very low, should not directly be reclaimed, it is necessary to its concentration is improved using simple economy method and is reclaimed again.
On 03 27th, 2013, Chinese invention patent application publication number CN102994771A was described a kind of from silver electrolysis
The method that palladium sponge is extracted in earth of positive pole parting liquid, major technique is to be enriched with palladium with palladium complex reaction using butyl xanthate, is used
Concentrated hydrochloric acid and hydrogen peroxide leaching, filtrate adds and is refined again after the heavy palladium of ammonium chloride, finally uses hydrazine hydrate reduction.The method is first
Need to consume the pH that alkali adjusts solution, the precipitating reagent butyl xanthate for then adopting is needed in higher temperature conditions（60~80℃）Under
Operation, butyl xanthate easily decomposes the toxic and harmfuls such as generation carbon disulfide, nitrogen oxides, hydrogen chloride, pollutes environment, is harmful to
The health of shop floor worker.
On October 21st, 2015, Chinese invention patent application publication number CN104988315A describes acid Palladium recovery work
Skill, method is with aqua regia dissolution palladium-containingmaterial material and denitration, with salt acid for adjusting pH to 1 ~ 1.5, after basic anionic resin absorption
Take off again and wash, dissolve, reducing the recovery for completing palladium.The complex processes such as nitre, acidity adjustment caught up with and there is aqua regia dissolution, high temperature in the technique,
Working condition is poor, serious to environmental hazard；Adsorbed using resin and taken off and washed, due to resin price is higher and also need acid/
Alkali makes resin regeneration, while regenerated liquid needs further to process so as to which overall operation is costly.
The content of the invention
The purpose of the present invention is the problem existed for above-mentioned prior art, proposes that one kind is high from silver anode slime parting liquid
The technique of effect green reclaim palladium.The method adopts Whote-wet method flow process, and using conventional equipment, technological operation is simple, and process need not catch up with
Nitre, the acid-base value without the need for adjusting original solution；The advantages of having little, the environmental friendliness of pollution, palladium recovery rate height and good quality simultaneously, fits
Close the research from Recover palladium in low concentration liquid containing palladium.
The purpose of the present invention is by the following means realizing：
The technique of efficient green Recover palladium in a kind of parting liquid from silver anode slime, it is characterised in that：With silver electrolysis anode slime as original
Material, through nitric acid parting is dissolved, and to the palladium and silver in parting liquid recovery extraction is carried out；The method contains following several stages：
Step 1：Parting liquid condensing crystallizing
Parting liquid is inserted in low-temperature evaporation crystallizer, excessively concentration is careful not to, to reduce palladium because carrying secretly with silver nitrate crystallization
Cause damage；When there are a large amount of silver nitrate crystals to generate, magma is gone to reservoir from crystallizer, be cooled to be filtered after room temperature
Separation of solid and liquid, gained silver nitrate crystal are washed 1 ~ 2 time, washing lotion and filtrate are mixed into concentrate, deliver to next process；Washing
Silver nitrate crystal afterwards adds hot water to carry out the silver-colored potroom process of dissolving return；
Step 2：The heavy silver washing of concentrate
Slightly excessive hydrochloric acid is added into concentrate and is stirred continuously carries out heavy silver, until producing without white precipitate as react eventually
Point；Stand and filtered after 1 ~ 2 h, the loss that filter residue hot wash is caused for 1 ~ 2 time with reduction silver chlorate to the absorption of palladium, as
The silver chlorate of filter residue returns silver smelting recovery and produces thick silver, and gained filtrate and washing lotion are mixed and send next procedure；
Step 3：Oxidation and heavy palladium
The mixed liquor of step 2 gained filtrate and washing lotion is placed in reactor, appropriate sodium chlorate is added and to be stirred continuously half little
When, to guarantee that palladium therein is all oxidized into Pd4+；Adding the ammonium chloride more excessive by 20% than theoretical amount carries out heavy palladium, stirring
After the h of reaction time 1, standing is filtrated to get the filter residue containing ammonium chloropalladate precipitation, and filter residue washs 1 ~ 2 with the ammonium chloride solution of saturation
Next procedure is sent after secondary, after filtrate and washing lotion mixing water process is sent；
Step 4：Removal of impurities is purified
The filter residue deionized water containing ammonium chloropalladate that step 3 is obtained is 3 by liquid solid product mass ratio:1mL/g holds in reaction
Mix in device, heating and simultaneously stirring dissolve it, until after red foam is wholly absent, being filtrated to get ammonium chloropalladite molten
Liquid, filter residue reclaims noble metal with pyrogenic process is returned after appropriate hot wash, and washing lotion pours heating in reaction vessel into after mixing with filtrate
To 85 ~ 90 DEG C, by 1：1 volume ratio adds chemical pure ammoniacal liquor, while stirring, controls terminal pH for 9 ~ 10；After solution clarification
Filter, be slowly added to the watery hydrochloric acid acidifying of configured 6 good mol/L, while mixing control solution acidifying terminal pH is 1, obtain
The ammonium network of faint yellow dichloro two Asia palladium precipitation, stands cooled and filtered, and the ammonium network of dichloro two Asia palladium precipitation washs two with dilute hydrochloric acid solution
Secondary rear deionized water is tuned into pasty state, and adds a certain amount of ammoniacal liquor to be stirred dissolving, till yellow mercury oxide disappears, obtains
The ammonia solution of the ammonium network of dichloro two Asia palladium；
Step 5：Metal Palladium is reduced and dried
At normal temperatures, to step（4）In the ammonia solution of gained dichloro two ammonium network Asia palladium, the hydrazine hydrate of 200 g/L is slowly added to, directly
When hydrazine hydrate is added in solution without significant reaction and solution transparent clear；Be filtrated to get Metal Palladium, Metal Palladium spend from
After sub- water washing under conditions of 150 ~ 180 DEG C drying to final products.
The silver chlorate of above-mentioned steps 2 returns silver smelting recovery and produces thick silver, is that silver nitride precipitation is returned into pyrogenic process system to reclaim.
The beneficial effects of the present invention is the following aspects：
（1）Silver electrolysis anode slime parting liquid is concentrated using low-temperature evaporation crystallization technique, efficiency high, obvious energy conservation；The method is not
The concentration raising that the palladium in parting liquid can only be made conveniently subsequently is reclaimed to it, after can also making silver nitrate with crystal habit precipitation
Dissolving returns silver-colored potroom and processes, and reduces precipitate A g+Required hydrochloric acid consumption；
（2）With sodium chlorate oxidation and to silver nitride precipitation hot wash, to reduce the loss of palladium, by the way that the acid of chlorine palladium is used in combination
The ammonium precipitation method and the palladium precipitation method refining of the ammino of dichloro two Asia obtain Metal Palladium product, and the method removes to greatest extent various impurity
Element, improves the recycling efficiency of palladium resource；
（3）The technique and simple to operate, environmental protection, it is to avoid the consumption of alkali and the high temperature of the butyl xanthate precipitation method catch up with nitre,
The complex processes such as roasting, it is practical, it is adaptable to the production practices of palladium are extracted in low concentration liquid containing palladium.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Specific embodiment
With reference to the accompanying drawings and detailed description to the present invention from efficient green Recover palladium in silver anode slime parting liquid
Technique is described in further detail.
Embodiment one
According to as shown in Figure 1 and such scheme process, by 0.5 m3The silver anode slime parting liquid containing the g/L of palladium 0.816 be placed in it is low
Condensing crystallizing in warm MVR crystallizing evaporators, reservoir is gone to when having a large amount of silver nitrate crystals to generate magma, is cooled to room temperature
After filter separation of solid and liquid, gained silver nitrate crystal washs the washing lotion after 2 times and mixes with filtrate, obtains containing the g/L's of palladium 1.243
Concentrate, returns silver-colored potroom and processes after silver nitrate crystal dissolving.Concentrated hydrochloric acid is added until silver all sedimentations, it is heavy to be filtrated to get
Silvering solution, and silver nitride precipitation is washed with hot water stirs, washing lotion mixes with heavy silvering solution.Add 30g/L sodium chlorate to be aoxidized, stir
Being directly added into according still further to 150g/L ammonium chlorides after half an hour carries out heavy palladium, filters and wash ammonium chloropalladate precipitation.It is complete with hot water
Dissolving ammonium chloropalladate, it is 9.0 that filtrate ammonia solvent adjusts pH, filters and adds the hydrochloric acid of 15 % to be acidified to pH and be in backward filtrate
1.0, the yellow mercury oxide for obtaining is washed with 5% watery hydrochloric acid, is redissolved with ammoniacal liquor after deionized water pulp, and it is 9.0 to adjust pH, mistake
Filter gained filtrate with the hydrazine hydrate reduction of 200 g/L, until reaction terminate and solution it is limpid it is transparent till, filtering drying is final to be obtained
To palladium product.The 99.89% of the palladium product purity that the process is obtained, the process palladium recovery rate is up to 85.2%.
Embodiment two
Silver anode slime parting liquid g/L containing palladium 0.931, the g/L containing palladium 1.522 Jing after the concentration of low temperature MVR crystallizing evaporators, other are former
Then flow process ibid example, the 99.92% of the palladium product purity for finally giving, the process palladium recovery rate is up to 86.5%.
Those of ordinary skill in the art should be understood：The specific embodiment of the present invention is the foregoing is only, and
The restriction present invention, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc. are not used in,
Should be included within protection scope of the present invention.
Claims (2)
1. in a kind of parting liquid from silver anode slime efficient green Recover palladium technique, it is characterised in that：It is with silver electrolysis anode slime
Raw material, through nitric acid parting is dissolved, and to the palladium and silver in parting liquid recovery extraction is carried out；The method contains following several stages：
Step 1：Parting liquid condensing crystallizing
Parting liquid is inserted in low-temperature evaporation crystallizer, excessively concentration is careful not to, to reduce palladium because carrying secretly with silver nitrate crystallization
Cause damage；When there are a large amount of silver nitrate crystals to generate, magma is gone to reservoir from crystallizer, be cooled to be filtered after room temperature
Separation of solid and liquid, gained silver nitrate crystal are washed 1 ~ 2 time, washing lotion and filtrate are mixed into concentrate, deliver to next process；Washing
Silver nitrate crystal afterwards adds hot water to carry out the silver-colored potroom process of dissolving return；
Step 2：The heavy silver washing of concentrate
Slightly excessive hydrochloric acid is added into concentrate and is stirred continuously carries out heavy silver, until producing without white precipitate as react eventually
Point；Stand and filtered after 1 ~ 2 h, the loss that filter residue hot wash is caused for 1 ~ 2 time with reduction silver chlorate to the absorption of palladium, as
The silver chlorate of filter residue returns silver smelting recovery and produces thick silver, and gained filtrate and washing lotion are mixed and send next procedure；
Step 3：Oxidation and heavy palladium
The mixed liquor of step 2 gained filtrate and washing lotion is placed in reactor, appropriate sodium chlorate is added and to be stirred continuously half little
When, to guarantee that palladium therein is all oxidized into Pd4+；Adding the ammonium chloride more excessive by 20% than theoretical amount carries out heavy palladium, stirring
After the h of reaction time 1, standing is filtrated to get the filter residue containing ammonium chloropalladate precipitation, and filter residue washs 1 ~ 2 with the ammonium chloride solution of saturation
Next procedure is sent after secondary, after filtrate and washing lotion mixing water process is sent；
Step 4：Removal of impurities is purified
The filter residue deionized water containing ammonium chloropalladate that step 3 is obtained is 3 by liquid solid product mass ratio:1mL/g holds in reaction
Mix in device, heating and simultaneously stirring dissolve it, until after red foam is wholly absent, being filtrated to get ammonium chloropalladite molten
Liquid, filter residue reclaims noble metal with pyrogenic process is returned after appropriate hot wash, and washing lotion pours heating in reaction vessel into after mixing with filtrate
To 85 ~ 90 DEG C, by 1：1 volume ratio adds chemical pure ammoniacal liquor, while stirring, controls terminal pH for 9 ~ 10；After solution clarification
Filter, be slowly added to the watery hydrochloric acid acidifying of configured 6 good mol/L, while mixing control solution acidifying terminal pH is 1, obtain
The ammonium network of faint yellow dichloro two Asia palladium precipitation, stands cooled and filtered, and the ammonium network of dichloro two Asia palladium precipitation washs two with dilute hydrochloric acid solution
Secondary rear deionized water is tuned into pasty state, and adds a certain amount of ammoniacal liquor to be stirred dissolving, till yellow mercury oxide disappears, obtains
The ammonia solution of the ammonium network of dichloro two Asia palladium；
Step 5：Metal Palladium is reduced and dried
At normal temperatures, to step（4）In the ammonia solution of gained dichloro two ammonium network Asia palladium, the hydrazine hydrate of 200 g/L is slowly added to, directly
When hydrazine hydrate is added in solution without significant reaction and solution transparent clear；Be filtrated to get Metal Palladium, Metal Palladium spend from
After sub- water washing under conditions of 150 ~ 180 DEG C drying to final products.
2. in a kind of parting liquid from silver anode slime according to claim 1 efficient green Recover palladium technique, its feature exists
Silver smelting recovery is returned in the silver chlorate of the step 2 and produce thick silver, be that silver nitride precipitation is returned into pyrogenic process system to reclaim.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107326396A (en) * | 2017-06-29 | 2017-11-07 | 郴州市金贵银业股份有限公司 | A kind of preparation method of silver electrolyte |
| CN108950234A (en) * | 2018-08-15 | 2018-12-07 | 大冶有色金属有限责任公司 | A method of separating platinum and palladium from platinum palladium mixture |
| CN109680154A (en) * | 2019-02-19 | 2019-04-26 | 核工业北京化工冶金研究院 | A method of gold-palladium is separated and recovered from dead catalyst |
| CN110592391A (en) * | 2019-09-19 | 2019-12-20 | 李旭意 | Method for purifying crude gold powder |
| CN110964917A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Palladium refining process |
| CN111218563A (en) * | 2020-02-17 | 2020-06-02 | 山东恒邦冶炼股份有限公司 | Method for efficiently recovering palladium from black gold powder |
| CN112662884A (en) * | 2020-12-16 | 2021-04-16 | 中国科学院电工研究所 | Method for recycling metallic silver in crystalline silicon heterojunction solar cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107326396A (en) * | 2017-06-29 | 2017-11-07 | 郴州市金贵银业股份有限公司 | A kind of preparation method of silver electrolyte |
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| CN110964917A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Palladium refining process |
| CN109680154A (en) * | 2019-02-19 | 2019-04-26 | 核工业北京化工冶金研究院 | A method of gold-palladium is separated and recovered from dead catalyst |
| CN110592391A (en) * | 2019-09-19 | 2019-12-20 | 李旭意 | Method for purifying crude gold powder |
| CN111218563A (en) * | 2020-02-17 | 2020-06-02 | 山东恒邦冶炼股份有限公司 | Method for efficiently recovering palladium from black gold powder |
| CN112662884A (en) * | 2020-12-16 | 2021-04-16 | 中国科学院电工研究所 | Method for recycling metallic silver in crystalline silicon heterojunction solar cell |
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Inventor after: Tan Lin Inventor after: Yuan Ninghui Inventor after: Huang Pengfei Inventor after: Jiang Chaojin Inventor before: Yuan Ninghui Inventor before: Huang Pengfei Inventor before: Tan Lin Inventor before: Jiang Chaojin |