CN104233370B - A kind of method utilizing copper-contained sludge to produce electrolytic copper - Google Patents
A kind of method utilizing copper-contained sludge to produce electrolytic copper Download PDFInfo
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Abstract
The present invention relates to a kind of method utilizing copper-contained sludge to produce electrolytic copper, belong to waste utilization field.The technical deficiency that traditional copper smelting by pyrometallurgy method exists that environmental pollution is large, copper content is not high in finished product, in order to overcome above-mentioned technical deficiency, the invention provides a kind of method utilizing copper-contained sludge to produce electrolytic copper, this technical process is to the less pollution of air, in the electrolytic copper product obtained, the content of copper can up to 99.99%, whole technique copper yield can reach more than 85%, therefore has broad application prospects.
Description
Technical field
The present invention relates to a kind of method utilizing copper-contained sludge to produce electrolytic copper, belong to waste utilization field.
Background technology
Along with the fast development of the industry such as electroplating industry, metal finishing industry, printed circuit board industry, create a large amount of copper-containing wastewater, at present, factory adopts neutralization precipitation process usually to this kind of waste water, thereby produce a large amount of copper-contained sludge, if this kind of mud is arbitrarily stacked, the probably stripping of the cupric ion in mud, and again enter water body or soil and cause secondary pollution.In addition; if copper arbitrarily abandons the significant wastage that certainly will cause resource as a kind of Nonrenewable resources; therefore carry forward vigorously recycling economy, copper-contained sludge is turned waste into wealth, reduce the development trend that environmental pollution is environmental protection technical field and even comprehensive utilization of resources field simultaneously.
In recent years, domestic and international scientific research personnel mainly adopts following three kinds of methods to copper-contained sludge recycling:
One is take blast furnace as the pyrotic smelting absorption method of representative: first carry out oven dry pre-treatment to copper-contained sludge, then with Wingdale, quartzite and fluorite for flux, high-temperature coal or coke are fuel or reductive agent, at high temperature carry out pyrotic smelting to copper-contained sludge and obtain blister copper.Although the method is through development and improve ripe day by day, there is the deficiencies such as energy consumption is high, environmental pollution is large, thus constrain applying of the method.Disclosed in Chinese patent CN100506727C " a kind of recycling treatment process of electroplating sludge ", electroplating sludge is dried by this technique, with flux, coke burden after enter smelting furnace melting and reclaim valuable metal.And for example Chinese patent CN102433437A disclosed " a kind of heavy metal-polluted mud resource and method for innocent treatment ", its treatment process steps: 1. pulp, slurry carries out deep dehydration to water ratio is less than 55%; 2. be 6%-12% by deep dehydration drying sludge to water ratio; 3. sludge-drying is added flux, binding agent carries out preparing burden, making block or pelletizing; 4. coke, fast material or pelletizing feed are put into smelting furnace melting and reclaim valuable metal.It is high all to there is energy consumption in above-mentioned two kinds of methods, and environment is unfriendly, and is unsuitable for the process of low levels heavy metal sewage sludge.
Two is chemical recyclings that sulfuric acid stirs acidleach: first in copper-contained sludge, add certain density sulphuric acid soln carries out agitation leach, question response terminates rear solid-liquid separation and obtains copper-containing solution, then adopts the methods such as sulfide precipitation, displacement, extraction electrodeposition to reclaim valuable metal copper.Disclosed in Chinese patent CN100402676C, " from electroplating sludge, reclaim the method for valuable metal ", it first uses Ore Leaching valuable metal to electroplating sludge, and solid-liquid separation after vulcanization acid sodium sinks copper, and then obtains liquid after cupric sulfide and heavy copper after solid-liquid separation.The method reaction times is shorter, and the Apparent leaching rate of copper is high, but sulfuric acid has stronger corrodibility, higher to reaction vessel requirement for anticorrosion, more fatal problem is that after sulfuric acid leaching, solid-liquid separation is extremely difficult because sludge components is complicated, Washing ratio extreme difference, the total yield of copper is low.
Three is calcining-acidleach absorption methods: calcined under the high temperature conditions by copper-contained sludge, allows most of impurity dissolve oxide compound slowly as iron, zinc, aluminium, nickel, silicon etc. are transformed into, copper is separated in ensuing process, finally with CuSO
4form reclaim.As Chinese Resources comprehensive utilization periodical phase December the 12nd in 2005 the 10th page, Li Hongyi quotes the researchs such as JitkaJandova and finds calcining acidleach absorption method, is carry out acidleach, calcining, acidleach process again to copper-contained sludge, finally reclaims with the form of mantoquita.The method flow process is simple, does not need to add other reagent, easy and simple to handle, but process energy consumption is higher, and the mantoquita of output is impure more.
Summary of the invention
Traditional copper smelting by pyrometallurgy method exists that environmental pollution is large, the high and technical deficiency that the content of elemental copper is not high of foreign matter content in finished product, in order to overcome above-mentioned technical deficiency, the invention provides a kind of method utilizing copper-contained sludge to produce electrolytic copper, this technical process is to the less pollution of air, in the product obtained, the high purity 99.99% of copper, therefore has broad application prospects.
The invention provides a kind of method utilizing copper-contained sludge to produce electrolytic copper, it specifically comprises the steps:
(1) sinter
:to be placed in differential sinter machine containing crystal water 80% bronze medal mud and sinter, sintering is until obtain cellular or particulate state agglomerate.
(2) oxygen-enriched side-blowing melting: by the cellular or particulate state agglomerate obtained in step (1), mix with quartzite, Wingdale and carbon, transfer to smelting furnace, the air continuing to pass into carrier of oxygen volume concentrations 90% is calcined, wherein calcining temperature is 1200-1250 DEG C, and oxygen-rich oxide blowing is to the mixture of the blister copper and matte that obtain copper content 85-95%; Wherein the consumption of quartzite is 6-8kg/tCu, the consumption of Wingdale is 3-4kg/tCu, the consumption of carbon is 10-12kg/tCu.Step (2) also comprises tail gas bag-type dust step.
(3) refining is turned round: the blister copper obtain step (2) and the mixture of matte are transferred in revolution refining furnace, quartzite, Wingdale, carbon and heavy oil is added in the mixture of blister copper and matte, in mixture, continue to pass into air calcine, wherein calcining temperature is 1100-1200 DEG C, and calcining obtains the anode copper coin of cupric 98%; Wherein the consumption of quartzite is 4-8kg/tCu, the consumption of Wingdale is 2-4kg/tCu, the consumption of carbon is 1-2kg/tCu, the consumption of heavy oil is 3-4kg/tCu.
(4) electrorefining: using the anode copper coin in step (3) as anode, pure copper flakiness is as negative electrode, the mixed solution of sulfuric acid and copper sulfate carries out reversible circulation electrolysis as electrolytic solution, and the temperature controlling electrolytic solution is 60-70 DEG C, and electrolysis obtains electrolytic copper of the present invention.Step also comprises the step adding flocculation agent in electrolytic solution in (4), and flocculation agent mass fraction is in the electrolytic solution 0.1%-0.3%; Further, flocculation agent is made up of natural polymer, polyvalent metal salt, acrylamide, vinylformic acid, urea; Further, flocculation agent is by natural polymer 5-50 part, polyvalent metal salt 1-5 part, acrylamide 60-90 part, and vinylformic acid 5-20 part, urea 0-5 part forms.Wherein natural polymer is at least one in chitin, starch and Mierocrystalline cellulose; Polyvalent metal salt is at least one in magnesium chloride, calcium chloride and aluminum chloride, and further, natural polymer is chitin, and polyvalent metal salt is aluminum chloride.
The present invention also provides a kind of preparation method of above-mentioned flocculation agent, natural polymer and polyvalent metal salt is comprised the steps: to dissolve at 50-70 DEG C, be cooled to radiation irradiation after room temperature, radiation dose is 50-100kGy, acrylamide, vinylformic acid and urea is added in solution, control polymerization temperature is 60-70 DEG C and carries out graft copolymerization outside the venue, can obtain flocculation agent of the present invention after having reacted.
Water content in cellular (or particulate state) agglomerate in step of the present invention (1) is when about 10-20%, and copper content is generally 20-50%.More post-treatment operations is conducive to when the water content of honeycomb clinker is at 10-20%, if the water content of honeycomb clinker is too low, not only make copper lose serious and reduce copper yield, and it is excessive to cause calcining rear Dust Capacity, is difficult to carry out smelting furnace process.
In step of the present invention (2), copper-contained sludge carries out also comprising tail gas bag-type dust step in sintering processes process in differential sinter machine, the tail gas be about to after calcining discharges after water-bath spraying again, so not only reduce the pollution to air, promote the environmental friendliness of calcining process, and the flue dust that bag-type dust obtains can be recovered to process in differential sinter machine again, thus turn avoid the loss of cupric waste.
Tradition copper smelting by pyrometallurgy is the industry of a high energy consumption high pollution, and a large amount of use air and coke, produce the discharge of oxynitride and oxysulfide further, can cause severe contamination to air.The innovative point of step of the present invention (2) is: first, oxygen-rich air (containing 90% oxygen) is passed in calcination process, because the space of furnace is larger, in fact the carrier of oxygen volume concentrations in furnace is 30-40%, effectively can reduce the existence of nitrogen like this, the discharge of oxynitride in agglomerate calcination process is greatly reduced, reduces the pollution of calcination process to air.The second, calcination process employs carbon, the use of carbon, make agglomerate calcination process sulphur oxide discharge reduce, reduce the pollution to air.The process of this process greatly reduces because copper smelting by pyrometallurgy is to the pollution of air, and wherein the discharge of oxynitride and oxysulfide reduces 80-90%.
In electrolytic refining course of copper, except main metallic copper is transferred to except negative electrode from anode, also along with gold and silver etc., some are insoluble to the metal of sulphuric acid soln to bottom of electrolytic tank sedimentation, it not only causes the decline of Cathode Copper Quality, and causes the loss of precious metal, therefore, the present invention adds flocculation agent in step (4) electrolytic process, after using this flocculation agent, electrolytic copper surface particle obviously reduces, and its chemical composition brings up to 99.99% by original copper content 99.95%.
The method utilizing copper-contained sludge to produce electrolytic copper of the present invention, compared with prior art has following excellent technical superiority:
1) the present invention is the invention of the improvement made from traditional copper smelting by pyrometallurgy technical foundation, its the most outstanding technical superiority is the combination of four steps of the present invention, namely drying, oxygen-enriched side-blowing melting, revolution refining and the combinationally using of electrorefining is sintered, adopt preparation method of the present invention directly can prepare electrolytic copper, its high purity 99.99%, the rate of recovery of copper is also more than 85%, and it to be significantly better than in prior art purity in disclosed copper mud recovery process and the rate of recovery.
2) traditional copper smelting by pyrometallurgy is the industry of a high energy consumption high pollution, and a large amount of use air and coke, produce the discharge of oxynitride and oxysulfide further, can cause severe contamination to air.Present invention process is by step 2) in tail gas cloth bag dedusting process is set and in step 3), uses oxygen-rich air and merge carbon and jointly calcine, make the discharge of oxynitride and oxysulfide reduce 80-90%, visible process environments friendliness of the present invention is improved greatly.
The present invention not only makes the precious metals such as the gold and silver in blister copper be reclaimed by the mode adding electrolytic solution flocculation agent in electrolytic refining course of copper, and the purity of cathode copper is improved greatly.
Embodiment
Specific embodiment is adopted to further illustrate content of the present invention below.
Following content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Embodiment 1, the present invention utilize copper-contained sludge to produce the method for electrolytic copper:
(1) sinter
:to be placed in differential sinter machine containing crystal water 80% bronze medal mud and sinter, sintering is until obtain cellular or particulate state agglomerate.
(2) oxygen-enriched side-blowing melting: by the cellular or particulate state agglomerate obtained in step (1), mix with 7kg/tCu quartzite, 4kg/tCu Wingdale and 11kg/tCu carbon, transfer to smelting furnace, the air continuing to pass into carrier of oxygen volume concentrations 90% is calcined, wherein calcining temperature is 1250 DEG C, and oxygen-rich oxide blowing is to the mixture of the blister copper and matte that obtain copper content 95%.
(3) refining is turned round: the blister copper obtain step (2) and the mixture of matte are transferred in revolution refining furnace, 6kg/tCu quartzite, 3kg/tCu Wingdale, 2kg/tCu carbon and 4kg/tCu heavy oil is added in the mixture of blister copper and matte, in mixture, continue to pass into air calcine, wherein calcining temperature is 1200 DEG C, and calcining obtains the anode copper coin of cupric 98%.
(4) electrorefining: using the anode copper coin in step (3) as anode, pure copper flakiness is as negative electrode, the mixed solution of sulfuric acid and copper sulfate carries out reversible circulation electrolysis as electrolytic solution, wherein in electrolytic solution, add flocculation agent, flocculation agent mass fraction is in the electrolytic solution 0.2%, flocculation agent is by chitin 25 parts, 3 parts, aluminum chloride dissolves at 60 DEG C, be cooled to radiation irradiation after room temperature, radiation dose is 80kGy, 75 parts of acrylamides are added in solution, 15 parts of vinylformic acid and 3 parts of urea, control polymerization temperature be 65 DEG C carry out outside the venue graft copolymerization obtain, the temperature controlling electrolytic solution is 65 DEG C, electrolysis obtains electrolytic copper of the present invention, its purity is 99.99%, the rate of recovery of copper is 85%.
Embodiment 2, the present invention utilize copper-contained sludge to produce the method for electrolytic copper:
(1) sinter
:to be placed in differential sinter machine containing crystal water 80% bronze medal mud and sinter, sintering is until obtain cellular or particulate state agglomerate.
(2) oxygen-enriched side-blowing melting: by the cellular or particulate state agglomerate obtained in step (1), mix with 6kg/tCu quartzite, 3kg/tCu Wingdale and 10kg/tCu carbon, transfer to smelting furnace, the air continuing to pass into carrier of oxygen volume concentrations 90% is calcined, wherein calcining temperature is 1200 DEG C, and oxygen-rich oxide blowing is to the mixture of the blister copper and matte that obtain copper content 89%.
(3) refining is turned round: the blister copper obtain step (2) and the mixture of matte are transferred in revolution refining furnace, 8kg/tCu quartzite, 4kg/tCu Wingdale, 1kg/tCu carbon and 4kg/tCu heavy oil is added in the mixture of blister copper and matte, in mixture, continue to pass into air calcine, wherein calcining temperature is 1100 DEG C, and calcining obtains the anode copper coin of cupric 98%.
(4) electrorefining: using the anode copper coin in step (3) as anode, pure copper flakiness is as negative electrode, the mixed solution of sulfuric acid and copper sulfate carries out reversible circulation electrolysis as electrolytic solution, wherein in electrolytic solution, add flocculation agent, flocculation agent mass fraction is in the electrolytic solution 0.1%, flocculation agent is by chitin 5 parts, 5 parts, aluminum chloride dissolves at 50 DEG C, be cooled to radiation irradiation after room temperature, radiation dose is 100kGy, 90 parts of acrylamides are added in solution, 20 parts of vinylformic acid, control polymerization temperature is 60 DEG C and carries out graft copolymerization outside the venue, reaction is obtained, the temperature controlling electrolytic solution is 60 DEG C, electrolysis obtains electrolytic copper of the present invention, its purity is 99.96%, the rate of recovery of copper is 76%.
Embodiment 3, the present invention utilize copper-contained sludge to produce the method for electrolytic copper:
(1) sinter
:to be placed in differential sinter machine containing crystal water 80% bronze medal mud and sinter, sintering is until obtain cellular or particulate state agglomerate.
(2) oxygen-enriched side-blowing melting: by the cellular or particulate state agglomerate obtained in step (1), mix with 8kg/tCu quartzite, 4kg/tCu Wingdale and 12kg/tCu carbon, transfer to smelting furnace, the air continuing to pass into carrier of oxygen volume concentrations 90% is calcined, wherein calcining temperature is 1250 DEG C, and oxygen-rich oxide blowing is to the mixture of the blister copper and matte that obtain copper content 90%.
(3) refining is turned round: the blister copper obtain step (2) and the mixture of matte are transferred in revolution refining furnace, 4kg/tCu quartzite, 2kg/tCu Wingdale, 2kg/tCu carbon and 3kg/tCu heavy oil is added in the mixture of blister copper and matte, in mixture, continue to pass into air calcine, wherein calcining temperature is 1200 DEG C, and calcining obtains the anode copper coin of cupric 98%.
(4) electrorefining: using the anode copper coin in step (3) as anode, pure copper flakiness is as negative electrode, the mixed solution of sulfuric acid and copper sulfate carries out reversible circulation electrolysis as electrolytic solution, wherein in electrolytic solution, add flocculation agent, flocculation agent mass fraction is in the electrolytic solution 0.3%, flocculation agent is by chitin 50 parts, 1 part, aluminum chloride dissolves at 70 DEG C, be cooled to radiation irradiation after room temperature, radiation dose is 50kGy, 60 parts of acrylamides are added in solution, 5 parts of vinylformic acid and 5 parts of urea, control polymerization temperature is 60-70 DEG C and carries out graft copolymerization outside the venue, reaction is obtained, the temperature controlling electrolytic solution is 60-70 DEG C, electrolysis obtains electrolytic copper of the present invention, its purity is 99.97%, the rate of recovery of copper is 79%.
Claims (7)
1. utilize copper-contained sludge to produce a method for electrolytic copper, it is characterized in that, comprise the steps:
(1) sinter: will be placed in differential sinter machine containing crystal water 80% bronze medal mud and sinter, sintering is until obtain cellular or particulate state agglomerate;
(2) oxygen-enriched side-blowing melting: by the cellular or particulate state agglomerate obtained in step (1), mix with quartzite, Wingdale and carbon, transfer to smelting furnace, the air continuing to pass into carrier of oxygen volume concentrations 90% is calcined, wherein calcining temperature is 1200-1250 DEG C, and oxygen-rich oxide blowing is to the mixture of the blister copper and matte that obtain copper content 85-95%;
(3) refining is turned round: the blister copper obtain step (2) and the mixture of matte are transferred in revolution refining furnace, quartzite, Wingdale, carbon and heavy oil is added in the mixture of blister copper and matte, in mixture, continue to pass into air calcine, wherein calcining temperature is 1100-1200 DEG C, and calcining obtains the anode copper coin of cupric 98%;
(4) electrorefining: using the anode copper coin in step (3) as anode, pure copper flakiness is as negative electrode, and the mixed solution of sulfuric acid and copper sulfate carries out reversible circulation electrolysis as electrolytic solution, and the temperature controlling electrolytic solution is 60-70 DEG C, and electrolysis obtains electrolytic copper;
Wherein, the step adding flocculation agent in electrolytic solution is also comprised in described step (4); Described flocculation agent massfraction is in the electrolytic solution 0.1%-0.3%;
Described flocculation agent is by natural polymer 5-50 part, and polyvalent metal salt 1-5 part, acrylamide 60-90 part, vinylformic acid 5-20 part, urea 0-5 part forms.
2. utilize copper-contained sludge to produce the method for electrolytic copper as claimed in claim 1, it is characterized in that, the consumption of the quartzite in described step (2) is 6-8kg/tCu, the consumption of Wingdale is 3-4kg/tCu, the consumption of carbon is 10-12kg/tCu.
3. utilize copper-contained sludge to produce the method for electrolytic copper as claimed in claim 1, it is characterized in that, described step (2) comprises tail gas bag-type dust step.
4. utilize copper-contained sludge to produce the method for electrolytic copper as claimed in claim 1, it is characterized in that, the consumption of the quartzite in described step (3) is 4-8kg/tCu, the consumption of Wingdale is 2-4kg/tCu, the consumption of carbon is 1-2kg/tCu, the consumption of heavy oil is 3-4kg/tCu.
5. utilize copper-contained sludge to produce the method for electrolytic copper as claimed in claim 1, it is characterized in that, described natural polymer is at least one in chitin, starch and Mierocrystalline cellulose; Described polyvalent metal salt is at least one in magnesium chloride, calcium chloride and aluminum chloride.
6. utilize copper-contained sludge to produce the method for electrolytic copper as claimed in claim 5, it is characterized in that, described natural polymer is chitin; Described polyvalent metal salt is aluminum chloride.
7. as claim 1 or claim 5 or the method utilizing copper-contained sludge to produce electrolytic copper according to claim 6, it is characterized in that, the preparation method of described flocculation agent comprises the steps: natural polymer and polyvalent metal salt to dissolve at 50-70 DEG C, be cooled to radiation irradiation after room temperature, radiation dose is 50-100kGy, acrylamide, vinylformic acid and urea is added in solution, control polymerization temperature is 60-70 DEG C and carries out graft copolymerization outside the venue, obtains flocculation agent after having reacted.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106400051A (en) * | 2016-11-23 | 2017-02-15 | 肇庆市飞南金属有限公司 | Method for achieving copper, nickel and tin separation through low-copper, high-nickel and high-tin anode electrolysis |
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| CN104789781A (en) * | 2015-03-27 | 2015-07-22 | 昆山市益民环保技术开发有限公司 | Processing method for comprehensive resource utilization of electroplating sludge and waste activated carbon |
| CN106757151A (en) * | 2016-11-23 | 2017-05-31 | 肇庆市飞南金属有限公司 | Cathode copper is produced using copper-contained sludge and separate the low energy consumption method of nickel, arsenic and tin |
| CN106498170A (en) * | 2016-11-23 | 2017-03-15 | 肇庆市飞南金属有限公司 | A kind of utilization copper-contained sludge produces the low energy consumption method of cathode copper |
| CN106929686B (en) * | 2017-04-10 | 2020-06-23 | 惠州Tcl环境科技有限公司 | Method for cooperatively recovering copper in ferric trichloride etching waste liquid by utilizing metal sludge |
| JP6816076B2 (en) * | 2017-11-29 | 2021-01-20 | パンパシフィック・カッパー株式会社 | How to make electrolytic copper |
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