CN105567986B - A kind of method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin - Google Patents
A kind of method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin Download PDFInfo
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- CN105567986B CN105567986B CN201511014055.9A CN201511014055A CN105567986B CN 105567986 B CN105567986 B CN 105567986B CN 201511014055 A CN201511014055 A CN 201511014055A CN 105567986 B CN105567986 B CN 105567986B
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- germanium
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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
- C22B7/04—Working-up slag
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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
- C22B41/00—Obtaining germanium
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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
- C22B58/00—Obtaining gallium or indium
-
- 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
Abstract
The invention discloses a kind of method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, comprise the following steps：A, with zinc electrolytic waste liquid, water and gallium germanium slag acidleach；B, by a step A pickle liquor iron replacement copper, displaced liquid is obtained；C, by above-mentioned displaced liquid tannin sinking germanium, it is filtrated to get germanium concentrate；D, by the alkali immersion liquid resin adsorption gallium germanium of the alkali leaching of acid leaching residue in step A, parsing sulfuric acid is added, the desorbed solution of germanium containing gallium is obtained, the sodium hydroxide added in desorbed solution, after control pH value reacts heavy gallium, is filtrated to get liquid after gallium concentrate and heavy gallium；E, after the heavy gallium that set-up procedure D is obtained liquid pH value, add magnesium sulfate, react heavy germanium, filter to obtain germanium concentrate.The present invention is reduced the acidleach leaching rate of gallium germanium by adjusting acidleach condition, improves gallium germanium alkali leaching leaching rate, resin adsorption gallium germanium, sulfuric acid solution parsing are used in alkali immersion liquid, then is neutralized with alkali, obtains gallium concentrate and germanium aqueous slkali, germanium aqueous slkali uses sulfuric acid magnesium precipitate again.
Description
Technical field
The present invention relates to a kind of method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, belongs to dissipated metal metallurgy
Field.
Background technology
Gallium is a kind of dissipated metal, and the concentration in the earth's crust is very low, and distribution is very extensive, is often scattered in nature with micro
In the ores such as bauxite, zincblende.Present primary gallium most in the world is all in the bayer liquor during producing aluminium
Recovery.The production of germanium is usually to utilize sulfuric acid leaching from flue dust caused by enrichment germanium oxide dust caused by zinc abstraction or germanic coal,
Tannin precipitation recovery.Have and contain gallium germanium in some zinc concentrates simultaneously, gallium germanium replacement slag, present conventional work are generated using zinc dust precipitation
Skill utilizes sulfuric acid leaching or pressure leaching, and the germanium of leachate germanium is then difficult to reclaim using tannin precipitation recovery, gallium.Patent No.
CN201410839448.2's《A kind of method of high efficiente callback germanium》The technique being combined using acidleach with alkali leaching, synthetical recovery
Gallium germanium, but the grade that the germanium in germanic acid magnesium be present is relatively low（5-10%）The problem of, follow-up distillation cost is higher.The present invention passes through tune
Whole acidleach condition reduces the acidleach leaching rate of gallium germanium, improves gallium germanium alkali leaching leaching rate, resin adsorption gallium germanium is used in alkali immersion liquid,
Sulfuric acid solution parses, then is neutralized with alkali, obtains gallium concentrate and germanium aqueous slkali, germanium aqueous slkali is used sulfuric acid magnesium precipitate, obtained germanic again
More than 20% germanium concentrate.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided one kind resin is from zinc dust precipitation gallium
The method that gallium germanium is reclaimed in germanium slag.
In order to solve the above technical problems, technical scheme proposed by the present invention is：
A kind of method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, comprises the following steps：
A, sized mixing with zinc electrolytic waste liquid, water and gallium germanium slag after acidleach, obtain acid leaching residue and a pickle liquor；
B, by a pickle liquor iron replacement copper caused by step A, iron powder addition is 1.2-1.5 times of amount of copper, instead
50-70 DEG C of temperature is answered, 1-2h is reacted, obtains displaced liquid and copper ashes；
C, by displaced liquid tannin sinking germanium caused by step B, tannin dosage is 25-30 times of germanium amount, reaction temperature 50-
70 DEG C, 10-60 minutes are reacted, are filtrated to get germanium concentrate；
D, by the alkali leaching of acid leaching residue in step A, the alkali immersion liquid resin adsorption gallium germanium after an alkali leaching, resin
Alkali dip amount of absorption is 20-100 times of resin volume, adds the parsing sulfuric acid that concentration is 0.05-2mol/l, obtains containing gallium
Germanium desorbed solution, the sodium hydroxide of concentration 10-25% is added in desorbed solution, after heavy gallium is reacted in control pH value 3.5-5.0, filtering
Obtain liquid after gallium concentrate and heavy gallium；
E, the pH value of liquid between 7.0-11.0, adds magnesium sulfate after the heavy gallium that set-up procedure D is obtained, and reacts heavy germanium, mistake
Filter to obtain germanium concentrate.
Further, an alkaline residue after an alkali leaching carries out secondary alkali leaching, and the secondary alkali immersion liquid that secondary alkali soaks to obtain is made
Match somebody with somebody liquid for an alkali leaching, the secondary alkali phase analysis that secondary alkali soaks to obtain enters in lead processing system.
The method according to claim 2 for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, it is characterised in that
Secondary alkali leaching is carried out with sodium hydroxide solution, its alkali leaching condition is liquid-solid ratio：5-10:1, reaction temperature：60-95 DEG C, react 1-
4h, terminal sodium hydrate content：20-100g/l.
In step D, carry out an alkali with sodium hydroxide solution and soak, its alkali leaching condition is liquid-solid ratio：5-10:1, reaction temperature
Degree：60-95 DEG C, react 1-4h, terminal sodium hydrate content：20-100g/l.
In step A, zinc electrolytic waste liquid, water and gallium germanium slag are sized mixing acidleach, 70-95 DEG C of controlling reaction temperature, and reaction 2-4 is small
When, terminal PH is 2.0-3.5.
Further, the germanium concentrate that above-mentioned reaction obtains enters in chlorinated distillation system.
In step E, add magnesium sulfate and 30-60 minutes are reacted into liquid after heavy gallium.
Compared with prior art, the advantage of the invention is that：
The method provided by the invention for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, by from the gallium germanium of zinc dust precipitation
Slag gallium adds water logging to go out first with zinc electrolytic waste liquid, and copper, zinc and part germanium are leached, and copper therein, germanium is separately recovered, and zinc returns
Return zinc generation system；Acid leaching residue is soaked with alkali twice again, and gallium and remainder germanium are leached, alkali immersion liquid passed through resin dedicated
(X900#) adsorption column, then gallium germanium is parsed with dilute sulfuric acid, the low gallium germanium desorbed solution of impurity is obtained, desorbed solution is replaced heavy gallium with alkali, sunk
Liquid sinks germanium with magnesium sulfate after gallium.
The present invention is reduced the acidleach leaching rate of gallium germanium by adjusting acidleach condition, gallium germanium alkali leaching leaching rate is improved, in alkali
Resin adsorption gallium germanium, sulfuric acid solution parsing are used in immersion liquid, then is neutralized with alkali, obtains gallium concentrate and germanium aqueous slkali, germanium aqueous slkali is again
With sulfuric acid magnesium precipitate, germanic more than 20% germanium concentrate is obtained.
By the inventive method, its rate of recovery is high, and gallium, the direct yield of germanium reach more than 90%, because using resin adsorption gallium germanium
Being separated with other compositions, gallium, germanium precipitation grade are high, reach 20-30%, simultaneously because because gallium germanium grade is high, successive refinements gallium germanium work
Skill is simple, and equipment investment is reduced, and greatly reduces production cost.
Brief description of the drawings
Fig. 1 is the theory structure schematic diagram of the present invention.
Embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
Limit the scope of the invention.
With reference to a kind of method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin shown in the drawings, including following work
Skill：
A, sized mixing with zinc electrolytic waste liquid, water and gallium germanium slag after acidleach, obtain acid leaching residue and a pickle liquor, operating condition：
The ratio of electrolysis waste solution and water=（1—4）：1
1. liquid-solid ratio：5-8:1
2. reaction temperature：70-95℃
3. the reaction time：2-4h
4. terminal pH value：2.0-3.5
B, a pickle liquor iron replacement copper, operating condition
1. iron powder addition：1.2-1.5 times of amount of copper
2. reaction temperature：50-70℃
3. the reaction time：1-2h
C, displaced liquid tannin sinking germanium, operating condition
1. tannin dosage：25-30 times of germanium amount
2. reaction temperature：50-70℃
3. the reaction time：10-60 minutes
D, by the alkali leaching of acid leaching residue in step A, heavy gallium, operating condition
1. liquid-solid ratio：5-8:1
2. reaction temperature：60-95℃
3. the reaction time：1-3h
4. terminal sodium hydrate content：10-40g/l
An alkaline residue after alkali leaching carries out secondary alkali leaching, operating condition
1. liquid-solid ratio：5-10:1
2. reaction temperature：60-95℃
3. the reaction time：1-4h
4. terminal sodium hydrate content：20-100g/l
The secondary alkali immersion liquid that secondary alkali soaks to obtain matches somebody with somebody liquid as an alkali leaching, and the secondary alkali phase analysis that secondary alkali soaks to obtain enters
In lead processing system；
Resin (X900#) adsorbs an alkali immersion liquid gallium germanium, operating condition
1. resin adsorption reduction of feed volume：20-100 times of resin volume
2. parse sulfuric acid concentration：0.05-2mol/l
3. naoh concentration：10—25%
4. absorption, parsing flow rate of liquid：2-5 times of resin volume/h
The desorbed solution of germanium containing gallium is obtained after operation, adds sodium hydroxide in desorbed solution, controls pH value 3.5-5.0, during reaction
Between 30-60 minutes sink gallium after, be filtrated to get liquid after gallium concentrate and heavy gallium；
E, liquid adds the heavy germanium of sulfuric acid reactive magnesium, operating condition after heavy gallium
1. pH value is in 7.0-11.0
2. with the heavy germanium of 10-25 times of magnesium sulfate of germanium amount, reaction time:30-60 minutes
Entered by germanium concentrate caused by this method in chlorinated distillation system.
With reference to above-mentioned concrete technology, it is as follows to implement three embodiments：
Raw material：Gallium germanium slag ingredient is shown in Table 1
The gallium germanium slag ingredient table of table 1（%）
Concrete operations condition：
Acidleach adds water to match somebody with somebody liquid using electrolysis waste solution, and secondary alkali leaching naoh concentration used is 30-50g/l, all anti-
All it should be carried out in 50 cubes of mechanic whirl-nett reaction grooves, filter press press filtration, for other conditions all as described in description of the process, each operation is molten
Liquid and slag specimen result see below Lie Gebiao：
A, acidleach, 10 tons of 35 cubes of gallium germanium slag zinc electrolytic waste liquids are sized mixing with 5 cubes of water, 70-95 DEG C of controlling reaction temperature,
2-4 hours are reacted, terminal PH is 2.0-3.5.Filtrate component is shown in Table 2.
The pickle liquor component list of table 2（g/l）
B, a pickle liquor iron replacement copper, iron powder addition are 1.25 times of amount of copper, reaction temperature：50-70 DEG C,
React 1-2h.
C, displaced liquid tannin sinking germanium, tannin dosage：24 times of germanium amount, reaction temperature：50-70 DEG C, 10-60 points of reaction
Clock, tannin sinking germanium slag is germanic to be respectively：Implementation column 1：3.24%, implementation column 2:2.98%；Implementation column 3:3.64%.
D, an alkali leaching, liquid-solid ratio：5-8:1, reaction temperature：60-95 DEG C, react 1-3h, terminal sodium hydrate content：
20-40g/l.One time alkali bath constituents are shown in Table 3：
3 alkali bath constituents tables of table（g/l）
Secondary alkali leaching, liquid-solid ratio：5-10:1, reaction temperature：60-95 DEG C, react 1-4h, terminal sodium hydrate content：20-
100g/l.Secondary alkali leaching composition is shown in Table 4：
4 two alkali bath constituents tables of table（g/l）
Resin (X900#) adsorbs an alkali immersion liquid gallium germanium, 4 cubes of resin adsorption feed liquids, parses sulfuric acid concentration：0.5mol/
L, 9 cubes of dosage, regenerate concentration of lye：1.0mol/lNaOH, 6 cubes of dosage, absorption, parsing and recovering liquid flow velocity：10 is vertical
Side/hour, the alkali immersion liquid resin adsorption gallium germanium after alkali leaching of concrete operations, alkali dip amount of resin adsorption are
20-100 times of resin volume, the parsing sulfuric acid that concentration is 0.05-2mol/l is added, the desorbed solution of germanium containing gallium is obtained, in desorbed solution
The middle sodium hydroxide for adding concentration 10-25%, control after heavy gallium is reacted in pH value 3.5-5.0, be filtrated to get gallium concentrate and heavy gallium
Liquid afterwards.Desorbed solution composition is shown in Table 5：
The desorbed solution component list of table 5（g/l）
E, the pH value of liquid between 7.0-11.0, adds magnesium sulfate after the heavy gallium that set-up procedure D is obtained, and reacts heavy germanium, mistake
Filter to obtain germanium concentrate.Liquid and gallium, germanium concentrate composition are shown in Table 7 after heavy gallium germanium：
Table 6 sinks liquid and gallium, germanium concentrate component list after gallium germanium（g/l）
Above-mentioned simply presently preferred embodiments of the present invention, not makees any formal limitation to the present invention.It is although of the invention
It is disclosed above with preferred embodiment, but it is not limited to the present invention.Therefore, it is every without departing from technical solution of the present invention
Content, according to the technology of the present invention essence to any simple modifications, equivalents, and modifications made for any of the above embodiments, it all should fall
In the range of technical solution of the present invention protection.
Claims (7)
- A kind of 1. method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, it is characterised in that comprise the following steps：A, sized mixing ratio=1-4 of acidleach, zinc electrolytic waste liquid and water with zinc electrolytic waste liquid, water and gallium germanium slag：1, obtain acid leaching residue With a pickle liquor；B, by a pickle liquor iron replacement copper caused by step A, iron powder addition is 1.2-1.5 times of amount of copper, and reaction is warm 50-70 DEG C of degree, 1-2h is reacted, obtains displaced liquid and copper ashes；C, by displaced liquid tannin sinking germanium caused by step B, tannin dosage is 25-30 times of germanium amount, reaction temperature 50-70 DEG C, 10-60 minutes are reacted, are filtrated to get germanium concentrate；D, by the alkali leaching of acid leaching residue in step A, the alkali immersion liquid resin adsorption gallium germanium after an alkali leaching, resin adsorption Alkali dip amount is 20-100 times of resin volume, adds the parsing sulfuric acid that concentration is 0.05-2mol/l, obtains the solution of germanium containing gallium Liquid is analysed, the sodium hydroxide of concentration 10-25% is added in desorbed solution, after heavy gallium is reacted in control pH value 3.5-5.0, is filtered Liquid after to gallium concentrate and heavy gallium；E, the pH value of liquid between 7.0-11.0, adds magnesium sulfate after the heavy gallium that set-up procedure D is obtained, and reacts heavy germanium, filters Germanium concentrate.
- 2. the method according to claim 1 for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, it is characterised in that one An alkaline residue after secondary alkali leaching carries out secondary alkali leaching, and the secondary alkali immersion liquid that secondary alkali soaks to obtain matches somebody with somebody liquid as an alkali leaching, secondary The secondary alkali phase analysis that alkali soaks to obtain enters in lead processing system.
- 3. the method according to claim 2 for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, it is characterised in that use Sodium hydroxide solution carries out secondary alkali leaching, and its alkali leaching condition is liquid-solid ratio：5-10:1, reaction temperature：60-95 DEG C, react 1- 4h, terminal sodium hydrate content：20-100g/l.
- 4. the method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin according to right will go 1, it is characterised in that step In rapid D, carry out an alkali with sodium hydroxide solution and soak, its alkali leaching condition is liquid-solid ratio：5-10:1, reaction temperature：60-95 DEG C, React 1-4h, terminal sodium hydrate content：20-100g/l.
- 5. the method according to claim 1 for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, it is characterised in that step In rapid A, zinc electrolytic waste liquid, water and gallium germanium slag are sized mixing acidleach, and 70-95 DEG C of controlling reaction temperature reacts 2-4 hours, and terminal PH is 2.0-3.5。
- 6. the method according to claim 1 for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, it is characterised in that anti- The germanium concentrate that should be obtained enters in chlorinated distillation system.
- 7. the method according to claim 1 for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin, it is characterised in that step In rapid E, add magnesium sulfate and 30-60 minutes are reacted into liquid after heavy gallium.
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| CN106086481B (en) * | 2016-08-23 | 2018-08-24 | 王朋 | A method of germanium in the germanic waste liquid of recycling |
| CN112410570B (en) * | 2020-11-11 | 2022-06-17 | 广东先导稀材股份有限公司 | Method for recovering gallium and germanium from gallium and germanium material |
| CN112626341A (en) * | 2020-12-11 | 2021-04-09 | 广东先导稀材股份有限公司 | Method for recovering gallium and germanium from gallium and germanium material |
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| CN102560133A (en) * | 2012-02-29 | 2012-07-11 | 北京矿冶研究总院 | Method for extracting gallium and germanium from zinc smelting slag |
| CN103882228A (en) * | 2013-12-20 | 2014-06-25 | 河南豫光锌业有限公司 | Method for enrichment and recovery of gallium and germanium from raffinate of indium smelting system |
| CN103695657A (en) * | 2013-12-24 | 2014-04-02 | 广西博士海意信息科技有限公司 | Method for enriching and recovering gallium and germanium from zinc hydrometallurgy waste residues |
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