CN108034823A - A kind of method that molybdenum and copper are recycled in the molybdenum removal slag from Tungsten smelting - Google Patents
A kind of method that molybdenum and copper are recycled in the molybdenum removal slag from Tungsten smelting Download PDFInfo
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- CN108034823A CN108034823A CN201711289681.8A CN201711289681A CN108034823A CN 108034823 A CN108034823 A CN 108034823A CN 201711289681 A CN201711289681 A CN 201711289681A CN 108034823 A CN108034823 A CN 108034823A
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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
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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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
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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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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Abstract
The present invention relates to a kind of method that molybdenum and copper are recycled in molybdenum removal slag from Tungsten smelting, comprise the following steps：Ball milling, Leaching Molybdenum, precipitation molybdenum, the process for leaching copper and copper electrodeposition, molybdenum removal slag passes through alkaline leaching molybdenum, molybdenum enters to leaching molybdenum liquid, copper realizes the separation of molybdenum and copper, leaching molybdenum liquid adds calcium chloride or calcium hydroxide precipitation molybdenum obtains molybdic acid calcium product in molybdenum slag is soaked, soak molybdenum slag and leach copper by pressure oxidation, copper-containing solution is obtained, copper-containing solution passes through electrodeposition, obtains cathode copper products.The advantages that this method has technology maturation, environmental-friendly, and metal recovery rate is high.
Description
Technical field
The present invention relates to non-ferrous metal field of hydrometallurgy, molybdenum and copper are recycled in especially a kind of molybdenum removal slag from Tungsten smelting
Method.
Background technology
Tungsten is valuable rare metal resources, because it is with fusing point is high, hardness is big, wear-resisting and corrosion-resistant etc. excellent performance
And it is used widely.In Tungsten smelting production process, the high tungsten product of purity is, it is necessary to carry out the pass such as tungsten separation in order to obtain
Key cleaning procedure.At present, the tungsten separation circuit of most Tungsten smelting enterprises uses selective precipitation, what this method produced
Sediment is mainly the mantoquita precipitation containing thiomolybdate, i.e. molybdenum removal slag.With the increasingly exhaustion of the mineral resources containing molybdenum, containing molybdenum two
The recycling of secondary resource increasingly earns widespread respect.
At present, handling the method for molybdenum removal slag has thermal process and wet processing, and the basic ideas of processing are all by molybdenum and copper
Realize separation, respectively obtain the leached mud of solution and cupric containing molybdenum, utilization is separately recovered so as to fulfill molybdenum and copper, current
Molybdenum removal slag processing method in, this technological process of generally existing is long, metal recovery rate is low, or even also there are SO2 atmosphere pollution etc.
Problem.
For example, Chinese patent notification number discloses time of molybdenum and copper in a kind of Tungsten smelting molybdenum removal slag for 104263955 A of CN
Receiving method, one, roasting that the method comprising the steps of, molybdenum removal slag is mixed with a certain amount of quick lime and is roasted after 580-600 DEG C of high temperature
20-50min is burnt, obtains material I；
Step 2: ball milling, resulting material I is carried out to be milled to 300-500 mesh, obtains material II；
Step 3: leaching, resulting material II is mixed with certain density dilute sulfuric acid, Leach reaction is carried out in 50-70 DEG C
40-90min, separation of solid and liquid is carried out by the material after Leach reaction, is collected filtrate and is obtained the leachate containing molybdenum and copper；
Step 4: extraction, gained leachate is mixed with the mixed extractant containing N235 and TBP and carries out hybrid extraction,
Collect hybrid extraction water mutually containing the copper-bath of copper, must both collect hybrid extraction organic phase and with a certain amount of ammonium hydroxide
Mixing is stripped, and is collected strip aqueous and is obtained ammonium molybdate solution；
Step 5: crystallization purifying, crystallization is evaporated by gained ammonium molybdate solution, must both be produced containing the ammonium paramolybdate of molybdenum
Product；
Find out from above step, the recovery method technological process of molybdenum and copper is long in the molybdenum removal slag and extraction and crystallization disappear
Of high cost, the tedious process of consumption.
The content of the invention
The purpose of the present invention is to solve defect existing in the prior art, there is provided one kind is recycled from Tungsten smelting molybdenum removal slag
The method of molybdenum and copper.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of method that molybdenum and copper are recycled in molybdenum removal slag from Tungsten smelting, comprises the following steps：
A, ball milling：Molybdenum removal slag obtains molybdenum removal slag fines after ball milling, classification；
B, Leaching Molybdenum：The molybdenum removal slag fines that step A is obtained is added by liquid-solid ratio with water and is mixed into leaching tanks, is stirred,
Alkaline solution Leaching Molybdenum is added, after leaching, separation of solid and liquid, obtains leaching molybdenum liquid and filter residue, filter residue are washed with water, and obtains wash water
With leaching molybdenum slag, wash water, which returns, leaches dispensing Leaching Molybdenum；
C, molybdenum is precipitated：Calcium chloride or calcium hydroxide are added into the leaching molybdenum liquid for obtaining step B, the molybdenum in leaching molybdenum liquid is sunk
Shallow lake forms molybdic acid calcium product；
D, copper is leached：The leaching molybdenum slag that step B is obtained is entered together with liquid after copper electrodeposition and sulfuric acid and is mixed with acid tank, and
While dispersant mixing is added, then be pumped into autoclave, the offer pressurization oxygen-enriched atmosphere into autoclave, pressurised oxygen in autoclave
Change and leach, flashed down discharge, separation of solid and liquid, obtains the copper leaching liquid of cupric；
E, copper electrodeposition：The copper leaching liquid of step D is pumped into copper electrodeposition process, leads to direct current electrodeposition production tough cathode, copper electricity
Liquid sends step D back to in acid tank after product, recycles.
Further, the technical data of Leaching Molybdenum is in step B：Liquid-solid ratio is 1/1-10/1, alkaline solution addition
For the 10%-100% of molybdenum removal slag quality, 10-100 DEG C of temperature, extraction time 30min-300min.
Further, the technical data of precipitation molybdenum is in step C：Calcium chloride or calcium hydroxide addition form molybdenum for molybdenum
1.0-3.0 times of theoretical amount needed for sour calcium, time 1-4h, 10-95 DEG C of temperature.
Further, the leaching process for copper technical parameter described in step D is：Acid concentration is 80-200g/L, liquid-solid ratio 5-
15：1,140-180 DEG C of temperature, partial pressure of oxygen 0.4-1.2MPa, reaction time 1-6h, dispersant dosage 0.5-4%, is leached
After the completion of, separation of solid and liquid, obtains copper leaching liquid.
Further, the parameter of the copper electrodeposition described in step E is：Tank voltage is 2.0-2.5V, 45-75 DEG C of temperature；Die opening
90-110mm；Acidity is 100-160g/L；Current density is 100-200A/m2, and electric effusion circular flow is 25-50L/min.
Further, the dispersant is sodium lignin sulfonate, one kind in calcium lignosulfonate.
Further, the size of molybdenum removal slag fine granules is -160 mesh in the step A.
Further, the step B neutral and alkalis solution is sodium hydroxide solution.
Beneficial effects of the present invention are：The molybdenum removal slag of this method passes through alkaline leaching molybdenum, and molybdenum enters to leaching molybdenum liquid, and copper is soaking
In molybdenum slag, the separation of molybdenum and copper is realized, leaching molybdenum liquid adds calcium chloride or calcium hydroxide precipitation molybdenum obtains molybdic acid calcium product, soaks molybdenum
Slag leaches copper by pressure oxidation, obtains copper-containing solution, copper-containing solution passes through electrodeposition, obtains cathode copper products.This method has
Technology maturation, environmental-friendly, the advantages that metal recovery rate is high.
Brief description of the drawings
Fig. 1 is the process flow chart of the present invention.
Embodiment
As shown in Figure 1, recycling the method for molybdenum and copper in a kind of molybdenum removal slag from Tungsten smelting, comprise the following steps：
A, ball milling：Molybdenum removal slag obtains molybdenum removal slag fines after ball milling, classification；
B, Leaching Molybdenum：The molybdenum removal slag fines that step A is obtained is added by liquid-solid ratio with water and is mixed into leaching tanks, is stirred,
Alkaline solution Leaching Molybdenum is added, after leaching, separation of solid and liquid, obtains leaching molybdenum liquid and filter residue, filter residue are washed with water, and obtains wash water
With leaching molybdenum slag, wash water, which returns, leaches dispensing Leaching Molybdenum；
C, molybdenum is precipitated：Calcium chloride or calcium hydroxide are added into the leaching molybdenum liquid for obtaining step B, the molybdenum in leaching molybdenum liquid is sunk
Shallow lake forms molybdic acid calcium product；
D, copper is leached：The leaching molybdenum slag that step B is obtained is entered together with liquid after copper electrodeposition and sulfuric acid and is mixed with acid tank, and
While dispersant mixing is added, then be pumped into autoclave, the offer pressurization oxygen-enriched atmosphere into autoclave, pressurised oxygen in autoclave
Change and leach, flashed down discharge, separation of solid and liquid, obtains the copper leaching liquid of cupric；
E, copper electrodeposition：The copper leaching liquid of step D is pumped into copper electrodeposition process, leads to direct current electrodeposition production tough cathode, copper electricity
Liquid sends step D back to in acid tank after product, recycles.
Further, the technical data of Leaching Molybdenum is in step B：Liquid-solid ratio is 1/1-10/1, alkaline solution addition
For the 10%-100% of molybdenum removal slag quality, 10-100 DEG C of temperature, extraction time 30min-300min.
Further, the technical data of precipitation molybdenum is in step C：Calcium chloride or calcium hydroxide addition form molybdenum for molybdenum
1.0-3.0 times of theoretical amount needed for sour calcium, time 1-4h, 10-95 DEG C of temperature.
Further, the leaching process for copper technical parameter described in step D is：Acid concentration is 80-200g/L, liquid-solid ratio 5-
15：1,140-180 DEG C of temperature, partial pressure of oxygen 0.4-1.2MPa, reaction time 1-6h, dispersant dosage 0.5-4%, is leached
After the completion of, separation of solid and liquid, obtains copper leaching liquid.
Further, the parameter of the copper electrodeposition described in step E is：Tank voltage is 2.0-2.5V, 45-75 DEG C of temperature；Die opening
90-110mm；Acidity is 100-160g/L；Current density is 100-200A/m2, and electric effusion circular flow is 25-50L/min.
Further, the dispersant is sodium lignin sulfonate, one kind in calcium lignosulfonate.
Further, the size of molybdenum removal slag fine granules is -160 mesh in the step A.
Further, the step B neutral and alkalis solution is sodium hydroxide solution.
Concrete operations embodiment is as follows：
A kind of chemical composition of typical Tungsten smelting molybdenum removal slag is shown in Table 1.
A kind of chemical composition of typical Tungsten smelting molybdenum removal slag of table 1, %
A, ball milling
Molybdenum removal slag chemical composition according to table 1, when tissue produces, below molybdenum removal slag ball milling, classification to -160 mesh,
Obtain molybdenum removal slag fines.
B, Leaching Molybdenum
During -160 mesh molybdenum removal slag fineves of step A are sent to leaching tanks, mixed, stirred, hydrogen-oxygen according to liquid-solid ratio 3/1
Change the weight that sodium adds and the 50% of weight is added for molybdenum removal slag, extraction temperature is 50 DEG C, and extraction time 2.0h, leaching terminates
Afterwards, separation of solid and liquid, obtains filtrate and filter residue, and filter residue is washed with water, and obtains wash water and leaching molybdenum slag, and wash water, which returns, leaches dispensing leaching
Molybdenum.Filtrate molybdenum concentration is 75g/L, and the leaching rate of molybdenum is more than 99%, and the loss of copper is less than 1%.
C, molybdenum is precipitated
Step B obtained filtrate send into precipitation tank to add the calcium chloride of heavy 2.5 times of molybdenum theoretical amount, sedimentation time 2h, sinks
Shallow lake temperature is 40 DEG C, and after precipitation, solid-liquor separation, obtains the sale of molybdic acid calcium product.
D, copper is leached
The leaching molybdenum slag that step B is obtained is sent in acid tank, according to liquid-solid ratio, liquid/sulfuric acid/water after electrodeposition is added, adjusts
It is 120g/L to leach beginning acid concentration, and it is 10/1 to leach liquid-solid ratio, while adds the sodium lignin sulfonate of leaching molybdenum slag weight 3%；Even
It is continuous to leach；Leaching condition is：Time 3h, 160 DEG C, partial pressure of oxygen 0.8MPa of temperature,
Pressure oxidation is leached in autoclave, and flashed down discharge, separation of solid and liquid, copper leaching liquid is sent to copper electrodeposition process.
E, copper electrodeposition
By the copper leaching liquid supplying sulfuric acid of step D to 140~150g/L, copper electrodeposition process is pumped into obtain cathode copper products,
The material parameters of copper electrodeposition process are：Tank voltage is 2.0~2.5V, 55~60 DEG C of temperature, and die opening is 90~110mm, electric current
Density is：100~200A/m2, electric effusion circular flow are 30~40L/min.Electrodeposition waste liquid, which is back to, leaches copper process conduct
Leaching agent recycles.
The molybdenum removal slag of this method passes through alkaline leaching molybdenum, and molybdenum enters to leaching molybdenum liquid, and copper realizes molybdenum and copper in molybdenum slag is soaked
Separation, leaching molybdenum liquid adds calcium chloride or calcium hydroxide precipitation molybdenum obtains molybdic acid calcium product, and leaching molybdenum slag is by pressure oxidation leaching
Copper, obtains copper-containing solution, and copper-containing solution passes through electrodeposition, obtains cathode copper products.This method has technology maturation, environmental-friendly,
The advantages that metal recovery rate is high.
Basic principle, main feature and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these change and
Improvement is both fallen within the range of claimed invention.The protection domain of application claims by appended claims and its
Equivalent defines.
Claims (8)
1. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting, it is characterised in that comprise the following steps：
A, ball milling：Molybdenum removal slag obtains molybdenum removal slag fines after ball milling, classification；
B, Leaching Molybdenum：The molybdenum removal slag fines that step A is obtained is added by liquid-solid ratio with water and is mixed into leaching tanks, is stirred, is added
Alkaline solution Leaching Molybdenum, after leaching, separation of solid and liquid, obtains leaching molybdenum liquid and filter residue, filter residue are washed with water, and obtains wash water and leaching
Molybdenum slag, wash water, which returns, leaches dispensing Leaching Molybdenum；
C, molybdenum is precipitated：Calcium chloride or calcium hydroxide are added into the leaching molybdenum liquid for obtaining step B, the molybdenum in leaching molybdenum liquid is precipitated shape
Into molybdic acid calcium product；
D, copper is leached：The leaching molybdenum slag that step B is obtained is entered together with liquid after copper electrodeposition and sulfuric acid and is mixed with acid tank, and at the same time
Addition dispersant mixes, then is pumped into autoclave, the offer pressurization oxygen-enriched atmosphere into autoclave, pressure oxidation leaching in autoclave
Go out, flashed down discharge, separation of solid and liquid, obtains the copper leaching liquid of cupric；
E, copper electrodeposition：The copper leaching liquid of step D is pumped into copper electrodeposition process, leads to direct current electrodeposition production tough cathode, after copper electrodeposition
Liquid sends step D back to in acid tank, recycles.
2. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting according to claim 1, it is characterised in that step
The technical data of Leaching Molybdenum is in B：Liquid-solid ratio is 1/1-10/1, and alkaline solution addition is the 10%- of molybdenum removal slag quality
100%, 10-100 DEG C of temperature, extraction time 30min-300min.
3. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting according to claim 1, it is characterised in that step
The technical data of precipitation molybdenum is in C：Calcium chloride or calcium hydroxide addition form theoretical amount needed for calcium molybdate for molybdenum
1.0-3.0 times, time 1-4h, 10-95 DEG C of temperature.
4. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting according to claim 1, it is characterised in that step
Leaching process for copper technical parameter described in D is：Acid concentration is 80-200g/L, liquid-solid ratio 5-15：1,140-180 DEG C of temperature, oxygen
Partial pressure is 0.4-1.2MPa, and reaction time 1-6h, dispersant dosage 0.5-4%, after the completion of leaching, separation of solid and liquid, is soaked
Copper liquid.
5. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting according to claim 1, it is characterised in that step
The parameter of copper electrodeposition described in E is：Tank voltage is 2.0-2.5V, 45-75 DEG C of temperature；Die opening 90-110mm；Acidity is 100-
160g/L；Current density is 100-200A/m2, and electric effusion circular flow is 25-50L/min.
6. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting according to claim 1 or 4, it is characterised in that
The dispersant is sodium lignin sulfonate, one kind in calcium lignosulfonate.
7. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting according to claim 1, it is characterised in that described
The size of molybdenum removal slag fine granules is -160 mesh in step A.
8. the method for molybdenum and copper is recycled in a kind of molybdenum removal slag from Tungsten smelting according to claim 1 or 2, it is characterised in that
The step B neutral and alkalis solution is sodium hydroxide solution.
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| CN201711289681.8A CN108034823A (en) | 2017-12-08 | 2017-12-08 | A kind of method that molybdenum and copper are recycled in the molybdenum removal slag from Tungsten smelting |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977672A (en) * | 2018-07-27 | 2018-12-11 | 成都虹波钼业有限责任公司 | A method of using molybdenum removal slag as waste iron molybdate |
| CN109252049A (en) * | 2018-11-16 | 2019-01-22 | 王水平 | A kind of alkaline leaching handles tungsten product molybdenum removal slag and recycles the process of molybdenum and copper |
| CN109338108A (en) * | 2018-11-16 | 2019-02-15 | 王水平 | A kind of wet-treating tungsten product molybdenum removal slag and the process for recycling molybdenum, copper, tungsten, sulphur |
| CN112899482A (en) * | 2021-01-15 | 2021-06-04 | 厦门钨业股份有限公司 | Treatment method of molybdenum removal slag |
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| CN102912135A (en) * | 2012-09-29 | 2013-02-06 | 崇义章源钨业股份有限公司 | Method for treating molybdenum removal slag |
| CN106756065A (en) * | 2016-12-14 | 2017-05-31 | 江西自立环保科技有限公司 | A kind of method of Recovering Copper ferronickel in matte from fuming furnace |
| CN107345275A (en) * | 2017-07-03 | 2017-11-14 | 信丰华锐钨钼新材料有限公司 | High efficiency extraction tungsten, molybdenum, the method for copper in a kind of slag from molybdenum |
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| CN101333598A (en) * | 2008-01-17 | 2008-12-31 | 郴州钻石钨制品有限责任公司 | Method for separating and extracting metallic tungsten and molybdenum from molybdenum removal slag generated by smelting tungsten |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977672A (en) * | 2018-07-27 | 2018-12-11 | 成都虹波钼业有限责任公司 | A method of using molybdenum removal slag as waste iron molybdate |
| CN108977672B (en) * | 2018-07-27 | 2020-09-25 | 成都虹波钼业有限责任公司 | Method for preparing iron molybdate by taking molybdenum-removing slag as raw material |
| CN109252049A (en) * | 2018-11-16 | 2019-01-22 | 王水平 | A kind of alkaline leaching handles tungsten product molybdenum removal slag and recycles the process of molybdenum and copper |
| CN109338108A (en) * | 2018-11-16 | 2019-02-15 | 王水平 | A kind of wet-treating tungsten product molybdenum removal slag and the process for recycling molybdenum, copper, tungsten, sulphur |
| CN112899482A (en) * | 2021-01-15 | 2021-06-04 | 厦门钨业股份有限公司 | Treatment method of molybdenum removal slag |
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Application publication date: 20180515 |