CN109023421A - A kind of purifying treatment method of silver electrolyte - Google Patents
A kind of purifying treatment method of silver electrolyte Download PDFInfo
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- CN109023421A CN109023421A CN201810929091.5A CN201810929091A CN109023421A CN 109023421 A CN109023421 A CN 109023421A CN 201810929091 A CN201810929091 A CN 201810929091A CN 109023421 A CN109023421 A CN 109023421A
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- silver
- silver electrolyte
- electrolyte
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- purifying treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
-
- 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
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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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
Abstract
The invention discloses a kind of purifying treatment methods of silver electrolyte, wherein comprising steps of silver electrolyte charcoal treated to be clean is removed the palladium in silver electrolyte；The silver electrolyte of charcoal treated is heated, it is 4 ~ 6 that silver oxide, which is then added, to pH, to carry out precipitation reaction, then removes precipitating to get the silver electrolyte after purified treatment.The present invention solves the problems, such as that the purifying treatment method apparatus and process requirement of existing silver electrolyte is complicated, can not effectively remove Metal Palladium.
Description
Technical field
The present invention relates to nonferrous metallurgy environmental technology field more particularly to a kind of purifying treatment methods of silver electrolyte.
Background technique
During electrolytic silver, the impurity such as copper, lead, antimony, bismuth, palladium, iron in anode plate can enter electrolyte, with silver-colored electricity
The extension of activity duration is solved, concentration of the impurity in silver electrolyte constantly increases and pollute electrolyte, this partial impurities can be with
Silver ion together cathode be precipitated, to influence the grade of electric silver powder.So how efficiently to purify removing waste silver electrolyte
In the impurity elements such as copper, lead, antimony, bismuth, palladium, iron be silver-colored electrolysis field a problem.
Currently, common silver electrolyte purifying method are as follows: crystallization-decomposition method, the salt precipitation method, displacement method, above method
The problem of concentration impurity ion is high although being able to solve in electrolyte, influences electric silver powder grade, above method is also deposited respectively
In nitrogen oxides pollution environment, energy consumption is high, the device is complicated, noble metal is lost the problems such as big, purification efficiency is low, and all can not
Metal Palladium is effectively removed, it is even more impossible to be recycled.
" method of the silver electrolyte except bismuth, antimony " of Chinese patent 00126155.X utilizes the nitrate of bismuth, antimony in Low acid
Under the conditions of the characteristic that hydrolyzes, the addition silver oxide and ammonium hydroxide of substep in silver electrolyte, by filtering can by the bismuth of precipitating, antimony into
Row recycling, filtrate can return to use after being adjusted again with nitric acid and silver nitrate.The method can only go out bismuth, antimony, cannot remove copper,
The impurity such as lead, iron, reaction process need to be added ammonium hydroxide, in penetrating odor, be unfavorable for the occupational health of employee.
Chinese invention patent CN1884623A also discloses a kind of " method of silver electrolyte purified treatment ", it is to utilize Ag
Hydrated ion Ag(OH is formed in aqueous solution)2 -, adjusting silver electrolyte pH value to be clean is 8 ~ 9, most in electrolyte
Pb, Cu, Bi, Sb are deposited in bottom of electrolytic tank in the form of hydroxide, after supernatant is filtered out with nitric acid adjust acidity after i.e.
It can return to silver electrolysis to use.Although this method has many advantages, such as that easy to operate, noble metal loss is small, the clarification time is short, should
Method cannot go out iron, palladium in electrolyte simultaneously, and clean-up effect can only achieve 10-2The g/L order of magnitude, compared with the present invention
It is relatively low compared with clean-up effect.
Chinese patent CN101113526A also discloses a kind of " method for purifying silver electrolytic solution during high-purity silver production process ",
Silver oxide is added in 90 DEG C of silver electrolyte to be clean, control reaction end pH value is 5.5 ~ 6, and can effectively go out silver electrolyte
The impurity such as middle copper, lead, iron, bismuth, antimony.It is higher that the method requires silver electrolyte to be clean that need to be heated to 90 DEG C of energy consumptions, Bu Neng
It is removed in purification process and extracts precious metal palladium.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of purified treatment sides of silver electrolyte
Method, it is intended to solve the purifying treatment method apparatus and process requirement complexity of existing silver electrolyte, Metal Palladium can not be effectively removed
Problem.
Technical scheme is as follows:
A kind of purifying treatment method of silver electrolyte, wherein comprising steps of
By silver electrolyte charcoal treated to be clean, the palladium in silver electrolyte is removed；
The silver electrolyte of charcoal treated is heated, it is 4 ~ 6 that silver oxide, which is then added, to pH, to carry out precipitation reaction, then is gone
Except precipitating, then solution acidity is adjusted to 7 ~ 10g/L to get the silver electrolyte after purified treatment.
The purifying treatment method of the silver electrolyte, wherein the heating temperature is 70 ~ 80 DEG C.
The purifying treatment method of the silver electrolyte, wherein the precipitation reaction time is 3 ~ 5h.
The purifying treatment method of the silver electrolyte, wherein precipitating is removed using the method being separated by solid-liquid separation.
The purifying treatment method of the silver electrolyte, wherein after the precipitation reaction further include a standing process, after standing
Precipitating is removed again.
The purifying treatment method of the silver electrolyte, wherein the standing process time is 8 ~ 10h.
The purifying treatment method of the silver electrolyte, wherein further comprise the steps of:
The silver electrolyte acidity after removal precipitating is adjusted to 7 ~ 10g/L using nitric acid.
The purifying treatment method of the silver electrolyte, wherein adjust silver electrolyte acidity using nitric acid.
The utility model has the advantages that being removed in the purifying treatment method of silver electrolyte provided by the present invention first with activated carbon adsorption
Precious metal palladium in silver electrolyte, reheats and silver oxide is added and adjust pH value to 4 ~ 6, with by precipitation reaction removing copper, lead,
The foreign metal ions such as antimony, bismuth, iron, treated in this way, and the concentration impurity ions such as silver electrolyte copper, lead, antimony, bismuth, iron, palladium can
It is down to 10-3For the g/L order of magnitude hereinafter, improving the purification efficiency of impurity element in electrolyte, nitre is added in purified silver electrolyte
After acid adjustment acidity, control certain concentration of silver ions, return silver-colored electrolysis system can output meet No. 1 silver of national standard, tool
Have good promotional value, and adsorb raw material of the active carbon as Recover palladium of palladium, can output meet national standard SM-Pd99.95 with
The palladium sponge of upper requirement solves the purifying treatment method apparatus and process requirement complexity of existing silver electrolyte, can not effectively go
The problem of except Metal Palladium.
Detailed description of the invention
Fig. 1 is the preferred embodiment flow chart of the purifying treatment method of silver electrolyte of the present invention.
Specific embodiment
The present invention provides a kind of purifying treatment method of silver electrolyte, to make the purpose of the present invention, technical solution and effect
Clearer, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
A kind of purifying treatment method of silver electrolyte of the present invention, wherein as shown in Figure 1, comprising steps of
S1, by silver electrolyte charcoal treated to be clean, remove the palladium in silver electrolyte；
S2, the silver electrolyte of charcoal treated is heated, then addition silver oxide to system pH is 4 ~ 6, anti-precipitate
It answers, then removes precipitating to get the silver electrolyte after purified treatment.
The purifying treatment method of silver electrolyte of the present invention, first with expensive in activated carbon adsorption removal silver electrolyte
Metal Palladium reheats and is added the pH to 4 ~ 6 of silver oxide to whole system, removes copper removal, lead, antimony, bismuth, iron to carry out precipitation reaction
Etc. foreign metal ions, so that obtaining the concentration impurity ions such as copper, lead, antimony, bismuth, iron, palladium is down to 10-3The g/L order of magnitude is below
Silver electrolyte after purified treatment.
Specifically, in the step S1, silver electrolyte to be clean is passed through into activated carbon adsorption bucket, passes through the knot of active carbon
Structure adsorptivity removes the palladium in electrolyte, while causing the loss of silver ion, nor affects on the removal of other subsequent metal ions,
And be adsorbed with raw material of the active carbon as Recover palladium of palladium, further purification production palladium sponge, can output meet national standard SM-
The palladium sponge of Pd99.95 requirements above had both realized the removal of palladium metal in silver electrolyte in this way, also achieved precious metal palladium
Recycling.
In the step S2, the silver electrolyte of charcoal treated is heated, silver oxide is then added and adjusts pH to big
In 4, it is preferable that regulation system pH to 4 ~ 6 is carried out, and consumes that nitric acid is opposite to lift system pH using silver oxide and nitric acid silver reaction,
Impurity metallic elements are made to generate hydroxide precipitating to get the silver electrolyte after purified treatment.Because of copper, lead, antimony, bismuth, iron etc.
The hydrolyzed PH value of impurity element is 4 ~ 6, pH to the too high waste that will cause silver oxide, and pH is too low then cannot complete precipitated impurities
Metal ion, the key reaction occurred are as follows:
Ag2O + 2HNO3 = 2AgNO3 + H2O
Cu2+ + 2OH- = Cu(OH)2↓
Fe(NO3)3+3H2O= Fe(OH)3↓+3HNO3
Pb(NO3)3+H2O= Pb(OH)2↓+2HNO3
Sb(NO3)3+2H2O =Sb(OH)2NO3↓+2HNO3
Bi(NO3)3+2H2O =Bi(OH)2NO3↓+2HNO3
When above-mentioned precipitation reaction carries out, it can be aided with and be stirred to react, and control in 3 ~ 5h, to accelerate precipitation reaction progress.
Preferably, the step S2 is carried out in enamel reaction still, and heating temperature is 70 ~ 80 DEG C, and temperature is too droning to form sediment instead
Should excessively slowly, and temperature it is excessively high it will cause moisture evaporation it is too fast, make whole system occur large change and influence reaction
It carries out, ultimately causes foreign metal ion removal and be not thorough.
In the step S2, after the completion of precipitation reaction, a period of time is stood, to allow precipitating to be sufficiently deposited on bottom；It is excellent
Selection of land stands 8 ~ 10h, such as 9h.The mode of separation of solid and liquid is recycled to remove precipitating to get purification is arrived after standing a period of time
Treated silver electrolyte, then the silver electrolyte nitric acid after the purified treatment is molten by the silver electrolyte adjustment after removal precipitating
Liquid acidity can return to silver-colored electrolysis system tissue production to 7 ~ 10g/L, 100 ~ 200g/L of concentration of silver ions, can output meet
The electric silver powder that No. 1 silver of national standard requires.
Below by embodiment, the present invention is described in detail.
Embodiment 1
Silver electrolyte to be clean (liquid referred to as to be clean) is taken, measures its foreign metal ion content, then the liquid to be clean is passed through
Active carbon adsorption barrel is crossed, the palladium in electrolyte is removed, the silver electrolyte of charcoal treated is added in enamel reaction still and is added
Then silver oxide is added to 75 DEG C to adjust pH to 5 after stirring 4h carries out precipitation reaction and stand 9h, then pass through separation of solid and liquid in heat
Removal precipitating is to get liquid 1 after purification；Take identical silver electrolyte to be clean to repeat the above steps 2 times, be purified rear liquid 2,
Liquid 3 after purification；After measurement purification after liquid 1, purification after liquid 2, purification in liquid 3 foreign metal ion content, 1 institute of result table
Show:
Table 1
| Cu | Pd | Pb | Bi | Sb | Fe | |
| Liquid (g/L) to be clean | 22.66 | 0.22 | 0.53 | 0.16 | 0.12 | 1.18 |
| Liquid 1(g/L after purification) | 0.0017 | 0.0005 | 0.001 | 0.001 | 0.001 | 0.001 |
| Liquid 2(g/L after purification) | 0.0019 | 0.0005 | 0.0027 | 0.001 | 0.001 | 0.001 |
| Liquid 3(g/L after purification) | 0.0016 | 0.0004 | 0.0067 | 0.001 | 0.001 | 0.001 |
Can be seen that treated by upper table, the concentration impurity ions such as silver electrolyte copper, lead, antimony, bismuth, iron, palladium can be down to 10- 3The g/L order of magnitude even hereinafter, illustrate the method for the invention can effectively remove the copper in silver electrolyte, lead, antimony, bismuth, iron,
The metal ions such as palladium.
As a comparison, the present embodiment utilize simultaneously copper displacement method and sulfuric acid precipitation method to same silver electrolyte to be clean into
Row experiment, the results are shown in Table 2:
Table 2
| Cu | Pd | Pb | Bi | Sb | Fe | |
| Liquid (g/L) to be clean | 22.66 | 0.22 | 0.53 | 0.16 | 0.12 | 1.18 |
| The method of the present invention (g/L) | 0.0017 | 0.0005 | 0.001 | 0.001 | 0.001 | 0.001 |
| Copper displacement method (g/L) | 24.52 | 0.16 | 0.048 | 0.12 | 0.08 | 0.86 |
| Sulfuric acid precipitation method (g/L) | 22.42 | 0.18 | 0.04 | 0.08 | 0.11 | 1.12 |
As can be seen that compared with copper displacement method and sulfuric acid precipitation method, method of the present invention in silver electrolyte copper, lead,
The foreign ions such as antimony, bismuth, iron, palladium can be effectively removed, and can be down to 10-3The g/L order of magnitude, greatly improves
Its removal rate.
In conclusion in a kind of purifying treatment method of silver electrolyte provided by the present invention provided by the invention, it is first sharp
With the precious metal palladium in activated carbon adsorption removal silver electrolyte, reheats and silver oxide adjusting pH value is added to 4 ~ 6, by heavy
Reaction of forming sediment removes copper, lead, antimony, bismuth, the foreign metal ions such as iron, treated in this way silver electrolyte copper, lead, antimony, bismuth, iron, palladium
Equal concentration impurity ions can be down to 10-3The g/L order of magnitude is hereinafter, improve the purification efficiency of impurity element in electrolyte, after purification
Silver electrolyte nitric acid adjustment acidity is added after, control certain concentration of silver ions return silver-colored electrolysis system can output meet national standard
It is required that No. 1 silver, there is good promotional value, and adsorb raw material of the active carbon as Recover palladium of palladium, can output meet state
The palladium sponge for marking SM-Pd99.95 requirements above, the purifying treatment method apparatus and process requirement for solving existing silver electrolyte are multiple
It is miscellaneous, the problem of Metal Palladium can not be effectively removed.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (8)
1. a kind of purifying treatment method of silver electrolyte, which is characterized in that comprising steps of
By silver electrolyte charcoal treated to be clean, the palladium in silver electrolyte is removed；
The silver electrolyte of charcoal treated is heated, it is 4 ~ 6 that silver oxide, which is then added, to pH, to carry out precipitation reaction, then is gone
Except precipitating is to get the silver electrolyte after purified treatment.
2. the purifying treatment method of silver electrolyte according to claim 1, which is characterized in that the heating temperature be 70 ~
80℃。
3. the purifying treatment method of silver electrolyte according to claim 1, which is characterized in that the precipitation reaction time is
3~5h。
4. the purifying treatment method of silver electrolyte according to claim 1, which is characterized in that using the method being separated by solid-liquid separation
Removal precipitating.
5. the purifying treatment method of silver electrolyte according to claim 1, which is characterized in that further include after the precipitation reaction
One stands process, removes precipitating again after standing.
6. the purifying treatment method of silver electrolyte according to claim 5, which is characterized in that the standing process time is
8~10h。
7. the purifying treatment method of silver electrolyte according to claim 1, which is characterized in that further comprise the steps of:
Silver electrolyte acidity after removal precipitating is adjusted to 7 ~ 10g/L.
8. the purifying treatment method of silver electrolyte according to claim 7, which is characterized in that adjust silver electrolysis using nitric acid
Liquid acidity.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149311A (en) * | 2018-01-09 | 2018-06-12 | 重庆立道表面技术有限公司 | Non-cyanide plating silvering solution purification method and device |
| CN112410828A (en) * | 2020-11-24 | 2021-02-26 | 深圳市贵金装备科技有限公司 | Process for preparing high-purity silver by high-concentration silver nitrate electrodeposition method |
| CN112479334A (en) * | 2020-10-27 | 2021-03-12 | 深圳市众恒隆实业有限公司 | Purification treatment method of silver electrolyte |
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| CN108149311A (en) * | 2018-01-09 | 2018-06-12 | 重庆立道表面技术有限公司 | Non-cyanide plating silvering solution purification method and device |
| CN112479334A (en) * | 2020-10-27 | 2021-03-12 | 深圳市众恒隆实业有限公司 | Purification treatment method of silver electrolyte |
| CN112410828A (en) * | 2020-11-24 | 2021-02-26 | 深圳市贵金装备科技有限公司 | Process for preparing high-purity silver by high-concentration silver nitrate electrodeposition method |
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