CN107435103A - A kind of method that efficient closed cycle of copper ashes utilizes - Google Patents

A kind of method that efficient closed cycle of copper ashes utilizes Download PDF

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Publication number
CN107435103A
CN107435103A CN201710530075.4A CN201710530075A CN107435103A CN 107435103 A CN107435103 A CN 107435103A CN 201710530075 A CN201710530075 A CN 201710530075A CN 107435103 A CN107435103 A CN 107435103A
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CN
China
Prior art keywords
copper ashes
sulfuric acid
utilizes
closed cycle
cupric
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Pending
Application number
CN201710530075.4A
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Chinese (zh)
Inventor
江亲义
曾斌
袁善禧
王焕华
胡亦发
郭红花
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Xinfeng Huarui Molybdenum New Materials Co Ltd
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Xinfeng Huarui Molybdenum New Materials Co Ltd
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Priority to CN201710530075.4A priority Critical patent/CN107435103A/en
Publication of CN107435103A publication Critical patent/CN107435103A/en
Pending legal-status Critical Current

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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
    • 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
    • C22B15/0084—Treating solutions
    • C22B15/0086—Treating solutions by physical methods
    • 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
    • C22B15/0084—Treating solutions
    • C22B15/0089—Treating solutions by chemical methods
    • C22B15/0091—Treating solutions by chemical methods by cementation
    • 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
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • 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 the method that a kind of efficient closed cycle of copper ashes utilizes, caused copper ashes carries out inorganic Ore Leaching after Tungsten smelting selective precipitation is reclaimed into tungsten, leach and complete, leached mud, which returns, leaches the secondary leaching of process, that leaches adjusts pH value 13 containing copper liquid, extracted again, it is 15 25% composite extractants (composite extractant of ketoxime and aldoxime) to extract organic phase composition, 75 85% sulfonated kerosenes, it is 1: 13: 1 compared to O/A controls, is extracted using three-level, one-level washing, two level is stripped, Cu in raffinate2+Less than 1g/L, inorganic Ore Leaching process is returned to after regeneration, Cu in strip liquor2+More than 40g/L, crystallization is evaporated, cupric sulfate pentahydrate is made, removed molybdenum process for Tungsten smelting selective precipitation, back extraction process is returned after crystalline mother solution regeneration.A closed cycle is formed using above-mentioned technique, efficiently utilizes copper ashes.

Description

A kind of method that efficient closed cycle of copper ashes utilizes
Technical field
The present invention relates to non-ferrous metal metallurgy waste material resource green extraction field, and in particular to a kind of copper ashes is efficiently closed circuit to follow The method that ring utilizes.
Background technology
Tungsten is important strategic metal, is referred to as " industrial tooth ", in national defence, military project, medicine equipment, Aero-Space There is very extensive application Deng field, and tungsten compound producing process, mainly extracted with ion exchange-selective precipitation, alkalescence Follow the example of as typical technique, wherein especially with the selective precipitation of Central South University Li Hong osmanthus teaching inventive, to the high-purity tungsten in China The progress of the preparation technique of compound serves the progradation of key.Selective precipitation is in ammonium tungstate solution after curing Mantoquita is added, in the form of Cu-Mo-S double salt, the molybdenum in ammonium tungstate and other impurity is co-precipitated, reach purification Purpose.The WO being co-precipitated in Cu-Mo-S double salt has been reclaimed3, after Mo, the copper ashes that leaves, generally in the form of coarse products outside Cupper smelting is sold to, added value is low, while the potential safety hazard of solid waste transportation be present.
The content of the invention
In view of the shortcomings of the prior art, the present invention is intended to provide the method that a kind of efficient closed cycle of copper ashes utilizes, passes through Inorganic Ore Leaching, pH value, extract and separate, evaporative crystallization, the technique of centrifuge dripping are adjusted, by the copper in copper ashes into five water sulfuric acid Copper, return to the selective precipitation for Tungsten smelting removes molybdenum process, realizes the efficient closed cycle of copper ashes on the spot and utilizes.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of method that efficient closed cycle of copper ashes utilizes, comprises the following steps：
S1 copper ashes sulfuric acid leachings, separation of solid and liquid after the completion of leaching obtain filter residue and cupric filtrate, and filter residue then participates in next Wheel handles sulfuric acid leaching link during copper ashes according to step S1-S5；
The cupric filtrate obtained in step S1 adjustment pH value is 1-3 by S2, stands 24h, and secondary filter is removed in filtrate Suspension, jelly, obtain cupric refined filtration liquid；
S3 is extracted the cupric refined filtration liquid obtained in S2, is extracted using three-level, one-level washing, two level back extraction；
The strip liquor obtained in step S3 is evaporated crystallization by S4, and crystallization is completed, and jacket water (J.W.) cold analysis goes out cupric sulfate pentahydrate；
S5 centrifuge drippings, what obtained cupric sulfate pentahydrate returned to Tungsten smelting selective precipitation removes molybdenum process, and obtains Crystalline mother solution regeneration, after supplementing appropriate sulfuric acid, as back washing agent, when participating in next round and handling copper ashes according to step S1-S5 Extracting and enriching copper ring section.
Further, in step S1, sulfuric acid concentration control be 2-4mol/L, and it is 2-4h that extraction time, which controls, extraction temperature Control as 323-353K, mixing speed control is 80-120r/min.
Further, in step S3, extracting organic phase composition is：The composite extractant of 15%-25% ketoximes and aldoxime and 75%-85% sulfonated kerosenes.
Further, in step S3, Cu in liquid phase2+Concentration control be 5-25g/L, extraction phase is controlled as 1 than O/A:1- 3:1。
Further, in step S3, Cu in raffinate2+Concentration be less than 1g/L, participate in next round after regeneration supplement sulfuric acid Sulfuric acid leaching link during copper ashes is handled according to step S1-S5, Cu is controlled in strip liquor2+More than 40g/L.
Further, in step S5, centrifuge speed is 800-1000r/min in the process of centrifuge dripping, dries the time Control as 40-60min.
The beneficial effects of the present invention are：The present invention develops a kind of efficient closed cycle Application way of copper ashes, main body work Skill is that inorganic Ore Leaching-tune pH- extract and separates-evaporative crystallization-centrifuge dripping produces cupric sulfate pentahydrate, wherein inorganic acid leaching slag Inorganic Ore Leaching process is returned, carries out secondary leaching, realizes the closed cycle of slag, in extract and separate, after raffinate supplement sulfuric acid, Inorganic Ore Leaching process is returned, as leaching agent, realizes closed cycle, evaporative crystallization mother liquor, after supplementing sulfuric acid, as back extraction Agent, closed cycle is realized, the cupric sulfate pentahydrate produced, return to selective precipitation and remove molybdenum process, realize closed cycle.
Embodiment
The invention will be further described below, it is necessary to which explanation, following examples are using the technical program before Carry, give detailed embodiment and specific operating process, but the scope of the present invention is not limited to the present embodiment.
A kind of method that efficient closed cycle of copper ashes utilizes, comprises the following steps：
S1 copper ashes sulfuric acid leachings, separation of solid and liquid after the completion of leaching obtain filter residue and cupric filtrate, and filter residue filter residue then participates in Next round handles sulfuric acid leaching link during copper ashes according to step S1-S5；
The cupric filtrate obtained in step S1 adjustment pH value is 1-3 by S2, stands 24h, and secondary filter is removed in filtrate Suspension, jelly, obtain cupric refined filtration liquid；
S3 is extracted the cupric refined filtration liquid obtained in S2, is extracted using three-level, one-level washing, two level back extraction；
The strip liquor obtained in step S3 is evaporated crystallization by S4, and crystallization is completed, and jacket water (J.W.) cold analysis goes out cupric sulfate pentahydrate；
S5 centrifuge drippings, what obtained cupric sulfate pentahydrate returned to Tungsten smelting selective precipitation removes molybdenum process, and obtains Crystalline mother solution regeneration, after supplementing appropriate sulfuric acid, as back washing agent, when participating in next round and handling copper ashes according to step S1-S5 Extracting and enriching copper ring section.
Further, in step S1, sulfuric acid concentration control be 2-4mol/L, and it is 2-4h that extraction time, which controls, extraction temperature Control as 323-353K, mixing speed control is 80-120r/min.
Further, in step S3, extracting organic phase composition is：The composite extractant of 15%-25% ketoximes and aldoxime and 75%-85% sulfonated kerosenes.
Further, in step S3, Cu in liquid phase2+Concentration control be 5-25g/L, extraction phase is controlled as 1 than O/A:1- 3:1。
Further, in step S3, Cu in raffinate2+Concentration be less than 1g/L, participate in next round after regeneration supplement sulfuric acid Sulfuric acid leaching link during copper ashes is handled according to step S1-S5, Cu is controlled in strip liquor2+More than 40g/L.
Further, in step S5, centrifuge speed is 800-1000r/min in the process of centrifuge dripping, dries the time Control as 40-60min.
Embodiment 1
1. caused copper ashes sulfuric acid leaching after Tungsten smelting selective precipitation recovery tungsten, sulfuric acid concentration control are 2mol/L, extraction time control are 2h, and extraction temperature control is 323K, and mixing speed control is 80r/min, leaches and completes, Gu Liquid separates, and cupric filtrate enters next process.Filter residue then participates in the sulfuric acid leaching link in the copper ashes processing of next round；
2. step 1. in obtain cupric filtrate adjustment pH value be 2, stand 24h, secondary filter remove filtrate in suspension Thing, jelly, obtain the refined filtration liquid of cupric；
3. extracting and enriching copper：2. the refined filtration liquid of the cupric obtained in is extracted, it is multiple for 20% to extract organic phase composition Close extractant (composite extractant of ketoxime and aldoxime), 80% sulfonated kerosene, Cu in liquid phase2+Concentration control is 20g/L, compared to O/ A controls are 2:1, extracted using three-level, one-level washing, two level back extraction.Contain Cu in raffinate2+0.8g/L, regenerate (supplement sulfuric acid), Participate in the sulfuric acid leaching process in the processing of next round copper ashes.Cu is controlled in strip liquor2+42g/L。
4. evaporative crystallization：3. the strip liquor obtained in is evaporated crystallization, crystallization is completed, and jacket water (J.W.) cold analysis goes out five water sulphur Sour copper.
5. centrifuge dripping：Centrifuge speed is 900r/min, and drying time control is 50min, obtained cupric sulfate pentahydrate Return to Tungsten smelting selective precipitation and remove molybdenum process, and obtained crystalline mother solution regeneration, after supplementing appropriate sulfuric acid, as anti- Extract agent and return to the extracting and enriching copper process participated in the processing of next round copper ashes, realize the overall closed cycle that copper ashes efficiently utilizes.
Embodiment 2
1. caused copper ashes sulfuric acid leaching after Tungsten smelting selective precipitation recovery tungsten, sulfuric acid concentration control are 3mol/L, extraction time control are 3h, and extraction temperature control is 353K, and mixing speed control is 120r/min, leaches and completes, Gu Liquid separates, and the filtrate of cupric enters next process, and filter residue then participates in the sulfuric acid leaching link in the copper ashes processing of next round；
2. adjust pH value：It is 3 by the filtrate adjustment pH value of 1. middle cupric, stands 24h, secondary filter removes the suspension in filtrate Thing, jelly, obtain the refined filtration liquid of cupric；
3. extracting and enriching copper, the refined filtration liquid of the cupric obtained in 2. is extracted.It is multiple for 25% to extract organic phase composition Close extractant (composite extractant of ketoxime and aldoxime), 75% sulfonated kerosene, Cu in liquid phase2+Concentration control is 25g/L, compared to O/ A controls are 3:1.Extracted using three-level, one-level washing, two level back extraction.Cu in raffinate2+0.6g/L, regenerate (supplement sulfuric acid), ginseng With the sulfuric acid leaching process in the processing of next round copper ashes.Cu is controlled in strip liquor2+48g/L；
4. evaporative crystallization, will 3. in obtain strip liquor and be evaporated crystallization, crystallization is completed, and jacket water (J.W.) cold analysis goes out five water sulfuric acid Copper.
5. centrifuge dripping：Centrifuge speed is 1000r/min, and drying time control is 40min, five obtained water sulfuric acid Copper, return to Tungsten smelting selective precipitation and remove molybdenum process, and obtained crystalline mother solution regeneration, after supplementing appropriate sulfuric acid, make The extracting and enriching copper process participated in the processing of next round copper ashes is returned for back washing agent, realizes that entirety that copper ashes efficiently utilizes is closed circuit and follows Ring.
Embodiment 3
1. caused copper ashes sulfuric acid leaching after Tungsten smelting selective precipitation recovery tungsten, the concentration control of sulfuric acid are 2mol/L, extraction time control are 3h, and extraction temperature control is 343K, and mixing speed control is 100r/min, after the completion of leaching Separation of solid and liquid, obtained cupric filtrate enter next process, and filter residue then participates in the sulfuric acid leaching in the copper ashes processing of next round Link；
2. adjust pH value：1. the filtrate adjustment pH value of middle cupric is 1,24h is stood, secondary filter removes the suspension in filtrate Thing, jelly, obtain the refined filtration liquid of cupric；
3. extracting and enriching copper, the refined filtration liquid of the cupric obtained in 2. is extracted.It is multiple for 15% to extract organic phase composition Close extractant (composite extractant of ketoxime and aldoxime), 85% sulfonated kerosene, Cu in liquid phase2+Concentration control is 15g/L, compared to O/ A controls are 1:1.Extracted using three-level, one-level washing, two level back extraction.Cu in raffinate2+0.9g/L, regenerate (supplement sulfuric acid), ginseng With the sulfuric acid leaching process in the processing of next round copper ashes.Cu is controlled in strip liquor2+41g/L；
4. evaporative crystallization, will 3. in obtain strip liquor and be evaporated crystallization, crystallization is completed, and jacket water (J.W.) cold analysis goes out five water sulfuric acid Copper.
5. centrifuge dripping, centrifuge speed 800r/min, drying time control are 60min, obtained cupric sulfate pentahydrate, Return to Tungsten smelting selective precipitation and remove molybdenum process, and obtained crystalline mother solution regeneration, after supplementing appropriate sulfuric acid, as anti- Extract agent, return to the extracting and enriching copper process participated in the processing of next round copper ashes, realize the overall closed cycle that copper ashes efficiently utilizes.
For those skilled in the art, technical scheme that can be more than and design, provide various corresponding Change and deform, and all these change and deformation, should be construed as being included within the protection domain of the claims in the present invention.

Claims (6)

1. a kind of method that efficient closed cycle of copper ashes utilizes, it is characterised in that comprise the following steps：
S1 sulfuric acid leachings：Copper ashes sulfuric acid leaching, separation of solid and liquid after the completion of leaching obtain filter residue and cupric filtrate, and filter residue is then joined With next round according to sulfuric acid leaching link during step S1-S5 processing copper ashes；
The cupric filtrate obtained in step S1 adjustment pH value is 1-3 by S2, stands 24h, and secondary filter removes the suspension in filtrate Thing, jelly, obtain cupric refined filtration liquid；
S3 extracting and enriching copper：The cupric refined filtration liquid obtained in S2 is extracted, extracted using three-level, one-level is washed, and two level is anti- Extraction；
The strip liquor obtained in step S3 is evaporated crystallization by S4, and crystallization is completed, and jacket water (J.W.) cold analysis goes out cupric sulfate pentahydrate；
S5 centrifuge drippings, what obtained cupric sulfate pentahydrate returned to Tungsten smelting selective precipitation removes molybdenum process, and obtained knot Brilliant mother liquor regeneration, after supplementing appropriate sulfuric acid, as back washing agent, participate in extraction when next round handles copper ashes according to step S1-S5 Take enriching Cu link.
2. the method that the efficient closed cycle of copper ashes according to claim 1 utilizes, it is characterised in that in step S1, sulfuric acid Concentration control be 2-4mol/L, extraction time control be 2-4h, and it is 323-353K that extraction temperature, which controls, and mixing speed, which controls, is 80-120r/min。
3. the method that the efficient closed cycle of copper ashes according to claim 1 utilizes, it is characterised in that in step S3, extraction Organic phase composition is：The composite extractant and 75%-85% sulfonated kerosenes of 15%-25% ketoximes and aldoxime.
4. the method that the efficient closed cycle of copper ashes according to claim 1 utilizes, it is characterised in that in step S3, liquid phase Middle Cu2+Concentration control be 5-25g/L, extraction phase is controlled as 1: 1-3: 1 than O/A.
5. the method that the efficient closed cycle of copper ashes according to claim 1 utilizes, it is characterised in that in step S3, raffinate Cu in liquid2+Concentration be less than 1g/L, sulfuric acid when next round handles copper ashes according to step S1-S5 is participated in after regeneration supplement sulfuric acid and is soaked Go out link, Cu is controlled in strip liquor2+More than 40g/L.
6. the method that the efficient closed cycle of copper ashes according to claim 1 utilizes, it is characterised in that in step S 5, centrifugation Centrifuge speed is 800-1000r/min in the process of drying, and drying time control is 40-60min.
CN201710530075.4A 2017-07-03 2017-07-03 A kind of method that efficient closed cycle of copper ashes utilizes Pending CN107435103A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110656244A (en) * 2019-09-23 2020-01-07 鲁西化工集团股份有限公司硅化工分公司 Organic silicon waste slurry hydrolysis residue treatment device, treatment technology and application
CN112063854A (en) * 2020-09-02 2020-12-11 河南豫光金铅股份有限公司 Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110656244A (en) * 2019-09-23 2020-01-07 鲁西化工集团股份有限公司硅化工分公司 Organic silicon waste slurry hydrolysis residue treatment device, treatment technology and application
CN112063854A (en) * 2020-09-02 2020-12-11 河南豫光金铅股份有限公司 Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material

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Application publication date: 20171205