CN102876903A - Direct acidity oxygen pressure leaching treatment method of crude tin copper removal residues - Google Patents
Direct acidity oxygen pressure leaching treatment method of crude tin copper removal residues Download PDFInfo
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- CN102876903A CN102876903A CN2012103774151A CN201210377415A CN102876903A CN 102876903 A CN102876903 A CN 102876903A CN 2012103774151 A CN2012103774151 A CN 2012103774151A CN 201210377415 A CN201210377415 A CN 201210377415A CN 102876903 A CN102876903 A CN 102876903A
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Abstract
Disclosed is a direct acidity oxygen pressure leaching treatment method of crude tin copper removal residues. The method includes that the crude tin copper removal residues containing 55-75% of tin and 8-18% of copper produced when liquid-state crude tin is added to sulphur to remove copper are leached for 4-6 hours and filtered to obtain a filtrate and residues with final acid of 46-118g/L under the conditions that the temperature is 120-150 DEG C, oxygen partial pressure is 0.15-0.25MPa and the initial acid is 100-250g/L, the residues are subjected to reduction smelting to produce crude tin, the filtrate is subjected to concentration, cooling and crystallization to produce a copper sulfate pentahydrate product or subjected to electrolysis to produce electrolytic copper, and a crystallization mother liquor or an electrolyzed solution is returned to a leaching process for dispensing liquids. By means of the direct acidity oxygen pressure leaching treatment method of the crude tin copper removal residues, tin and copper in the crude tin copper removal residues can be rapidly and efficiently separated, and waste water, waste gases and waste residues are not generated.
Description
Technical field
The present invention relates to smelting field of nonferrous metal, particularly a kind of thick tin is pressed except the direct acid oxygen of copper ashes and is leached treatment process.
Background technology
After the tin concentrate is sloughed most sulphur and arsenic through fluidized bed roasting, output tin calcining; The tin calcining is allocated the raw coal of going back of suitable proportion into, carries out retailoring in reverberatory furnace, electric furnace or Ausmelt furnace, the thick tin of output.In the retailoring process, the copper in the tin calcining is reduced to metallic copper, and is dissolved in reverberatory furnace, electric furnace or Ausmelt furnace in the liquid thick tin; Liquid thick tin adds sulphur and carries out copper removal in refining process, the slag of stanniferous 50～75%, the cupric 8～20% that produces during copper removal, and namely thick tin also claims sulphur slag, S slag or copper ashes except copper ashes.Thick tin is three kinds of metallic tin, tin protoxide and cuprous sulfides except the main phase composition of copper ashes.
Thick tin contains 50～75% tin except in the copper ashes, therefore, reclaims thick tin except the tin in the copper ashes, and the economic and technical norms impact that whole tin is smelted is larger.Simultaneously, because thick tin contains 8～20% copper except in the copper ashes, therefore, reclaim thick tin except the tin in the copper ashes, at first be thick tin will be separated with copper except the tin in the copper ashes.
At present, thick tin mainly contains three kinds of techniques except the traditional treatment method of copper ashes, and the first is floatation process, and the second is sinter process, and the third is electrolysis process.
Adopt floatation process to process thick tin except copper ashes, mainly be to utilize thick tin to have hydrophobicity except the cuprous sulfide in the copper ashes, thick tin then has wetting ability except metallic tin and tin protoxide in the copper ashes, adding under flotation reagent and the venting condition, cuprous sulfide shows as flotability, enters the phase of swimming, and metallic tin and tin protoxide show as not flotability, enter in the mine tailing, thereby reached separating of tin and copper.But in production application, because thick tin is very thin except the tin protoxide in the copper ashes, in floatation process, there is the inferior tin of partial oxidation to be carried secretly by the bubble of upward movement and entered the phase of swimming, reduced the direct yield of tin, simultaneously in the slag the cuprous caking of partial vulcanization is arranged or wrapped up by metallic tin, can't when flotation, obtain enough buoyancy, do not enter the phase of swimming, but enter mine tailing, reduced the direct yield of copper, in floatation process, the direct yield of copper generally only has 65～75%, and the direct yield of tin also only has 80～85%; In addition, because floatation process has adopted flotation reagent and conditioning agent, flotation reagent has xanthate or black powder etc., and conditioning agent has sodium hydroxide, sodium sulphite etc., and production on-site environment is poor, and the part flotation waste water of output is difficult to process.Also have, the cuprous sulfide flotation concentrate that obtains need to pass through the processes such as roasting, leaching, crystallization or electrolysis treatment again, and technical process is long, and management difficulty is large, and production cost is high.
Adopt sinter process to process thick tin except copper ashes, except after copper ashes carries out oxidizing roasting with thick tin, make thick tin be oxidized to cupric oxide except the cuprous sulfide in the copper ashes, the oxidizing roasting product is in follow-up leaching, cupric oxide is entered solution by leaching and forms copper sulfate, and tin metal and oxide compound thereof are not leached, and are deposited in the leached mud, through after the solid-liquid separation, reached separating of tin and copper.This technique has advantages of that Production Flow Chart is short, the tin rate of recovery is high, does not externally discharge slag and effluent; But because thick tin removes the higher metallic tin that contains in the copper ashes, the fusing point of slag is very low, in roasting process, easily the knot kiln had both affected the normal operation of producing, and also directly reduced the oxidizing roasting effect of cuprous sulfide, therefore, the direct yield of copper is lower, generally only has 60～70%.In addition, because roasting process consumes the energy, production cost and energy consumption are higher.
Adopt electrolysis process to process thick tin except copper ashes, to utilize thick tin also can be dissolved in the silicofluoric acid electrolytic solution except the metallic state tin in the copper ashes has good electroconductibility, thick tin directly is dissolved in the silicofluoric acid electrolytic solution except the tin protoxide in the copper ashes, and thick tin is relatively poor and be not dissolved in the silicofluoric acid solution except the cuprous sulfide electroconductibility in the copper ashes, under the dc electrolysis condition, metallic state tin and tin protoxide dissolve and separate out at negative electrode, cuprous sulfide does not dissolve and enters in the anode sludge, thereby has reached separating of tin and copper.This technique have advantages of copper recovery high, fast reclaim tin, externally do not discharge slag and effluent; Its shortcoming is: 1. electrolytic process labour intensity is large, and all materials all need the employment frock to enter in the plastic compound bag, and electrolysis anode sludge needs manually to collect from plastic compound bag, and 2. the direct yield of electrolytic process tin is low, generally only has 40～50%; 3. the anode sludge has been carried the silicofluoric acid electrolytic solution secretly, and when follow-up roasting and retailoring, the cloth bag that can heavy corrosion gathers dust causes metal loss, and 4. technical process is long, and power consumption is large, and production cost is high.
Summary of the invention
The purpose of this invention is to provide a kind of thick tin and press except the direct acid oxygen of copper ashes and leach treatment process, the method can be efficiently, the thick tin of sharp separation is except tin and copper in the copper ashes, and not output waste water, waste gas and waste residue, effective protection of the environment.Have advantages of that technical process is short, tin and copper direct yield be high.
The present invention is achieved through the following technical solutions above-mentioned purpose: a kind of thick tin is pressed except the direct acid oxygen of copper ashes and is leached treatment process, comprises the steps:
(1) be that the thick tin of stanniferous 55～75%, the cupric 8～18% that will produce when the thick tin of liquid state adds the sulphur copper removal is except copper ashes, be that 120～150 ℃, oxygen partial pressure are 0.15～0.25MPa, the acid of beginning is under the condition of 100～250 grams per liters in temperature, leached 4～6 hours, filter, obtain filtrate and filter residue that whole acid is 46～118 grams per liters
(2) be to carry out 6 hours thick tin of output of retailoring under 1200～1260 ℃ the condition in temperature with filter residue,
(3) according to a conventional method filtrate is concentrated crystallisation by cooling separation of produced cupric sulfate pentahydrate product or carry out the electrolysis production electrolytic copper, liquid returns step (1) dosing after crystalline mother solution or the electrolysis.
Outstanding advantages of the present invention is:
Adopt the present invention can be efficiently, the thick tin of sharp separation removes tin and copper in the copper ashes, and process not output waste water, waste gas and waste residue have advantages of that technical process is short, tin and copper direct yield be high.
In leaching process, owing to having adopted acid oxygen to press leaching-out technique, namely directly oxygen is pressed leaching-out technique, thick tin is oxidized to cupric oxide except the cuprous sulfide in the copper ashes, cupric oxide further is dissolved in and becomes copper-bath in the dilution heat of sulfuric acid, and simultaneously, thick tin is oxidized to four stannic oxide except metallic tin and tin protoxide in the copper ashes, four stannic oxide are not dissolved in dilution heat of sulfuric acid, be deposited in the leached mud, through after the solid-liquid separation, copper has entered in the solution, tin is deposited in the slag, has realized separating of tin and copper.Owing to adopting direct oxygen to press leaching-out technique, the step of separating of tin and copper finishes, and has effectively shortened technical process; In addition, at leaching process, cuprous sulfide, metallic tin and tin protoxide degree of oxidation are thorough, therefore, the good separation of tin and copper, tin and copper all have higher direct yield, and the direct yield of copper surpasses 85%, and the direct yield of tin surpasses 99%.
Description of drawings
Fig. 1 is that thick tin of the present invention is pressed the process flow sheet that leaches treatment process except the direct acid oxygen of copper ashes.
Embodiment
Below by drawings and Examples technical scheme of the present invention is described further.
Embodiment 1
The present embodiment is the first example that thick tin of the present invention removes the treatment process of copper ashes, comprises the steps:
(1) acid oxygen is pressed and is leached: will be stanniferous 55%, the thick tin of cupric 18% removes 3 tons of copper ashes, the acid of add beginning is 15 cubic metres of the leach liquors of 100 grams per liters, be that 120 ℃, oxygen partial pressure are under the condition of 0.15MPa in temperature, in 20 cubic metres autoclave pressure, leached 6 hours; After leach finishing, filter, 14 cubic metres of the filtrates that the whole acid of output is 46 grams per liters, cupric 34 grams per liters, stanniferous 0.32 grams per liter, output is moisture 32%, stanniferous 70.3%, 3.5 tons of the filter residues of cupric 2.5%; The direct yield of copper is 88.1%, and the direct yield of tin is 99.7%
(2) filter residue retailoring: with 3.5 tons of filter residues, allocate into and go back 0.5 ton in raw coal, be 1250 ℃ in temperature and carried out retailoring 6 hours, produce 1.51 tons in the thick tin of stanniferous 92.6%, cupric 3.4%.
(3) the concentrated crystallisation by cooling of filtrate: with behind 14 cubic metres the concentrated crystallisation by cooling of filtrate, carry out centrifugation, 6.05 cubic metres of the crystalline mother solutions of 10.3 tons of output cupric 25.1% cupric sulfate pentahydrate products and cupric 35.4 grams per liters according to a conventional method; Crystalline mother solution returns oxygen and presses the leaching process dosing.
Embodiment 2
The present embodiment is the second example that thick tin of the present invention removes the treatment process of copper ashes, comprises the steps:
(1) acid oxygen is pressed and is leached: will be stanniferous 65%, the thick tin of cupric 13% removes 3 tons of copper ashes, the acid of add beginning is 15 cubic metres of the leach liquors of 150 grams per liters, be that 135 ℃, oxygen partial pressure are under the condition of 0.20MPa in temperature, in 20 cubic metres autoclave pressure, leached 5 hours; After leach finishing, filter, 13.8 cubic metres of the filtrates that the whole acid of output is 99 grams per liters, cupric 25 grams per liters, stanniferous 0.61 grams per liter, output is moisture 31%, stanniferous 74.3%, 3.8 tons of the filter residues of cupric 1.7%; The direct yield of copper is 88.4%, and the direct yield of tin is 99.8%.
(2) filter residue retailoring: with 3.8 tons of filter residues, allocate into and go back 0.5 ton in raw coal, be 1260 ℃ in temperature and carried out retailoring 6 hours, produce 1.82 tons in the thick tin of stanniferous 93.4%, cupric 2.3%.
(3) the concentrated crystallisation by cooling of filtrate: with behind 13.8 cubic metres the concentrated crystallisation by cooling of filtrate, carry out centrifugation, 4.9 cubic metres of the crystalline mother solutions of 6.9 tons of output cupric 25.0% cupric sulfate pentahydrate products and cupric 35.2 grams per liters according to a conventional method; Crystalline mother solution returns oxygen and presses the leaching process dosing.
Embodiment 3
The present embodiment is the 3rd example that thick tin of the present invention removes the treatment process of copper ashes, comprises the steps:
(1) acid oxygen is pressed and is leached: will be stanniferous 75%, the thick tin of cupric 8% removes 4 tons of copper ashes, the acid of add beginning is 16 cubic metres of the leach liquors of 150 grams per liters, be that 150 ℃, oxygen partial pressure are under the condition of 0.25MPa in temperature, in 20 cubic metres autoclave pressure, leached 4 hours; Finish after leaching, filter, 14.4 cubic metres of the filtrates that the whole acid of output is 118 grams per liters, cupric 20 grams per liters, stanniferous 0.72 grams per liter, output is moisture 30%, stanniferous 82.1%, 5.2 tons of the filter residues of cupric 0.88%; The direct yield of copper is 90.0%, and the direct yield of tin is 99.6%.
(2) filter residue retailoring: with 5.2 tons of filter residues, allocate into and go back 0.7 ton in raw coal, be 1250 ℃ in temperature and carried out retailoring 6 hours, produce 2.76 tons in the thick tin of stanniferous 94.5%, cupric 1.05%.
(3) the concentrated crystallisation by cooling of filtrate: with behind the concentrated crystallisation by cooling of the liquid of 14.4 cubic metres of filters, carry out centrifugation, 3.9 cubic metres of the crystalline mother solutions of 6.0 tons of output cupric 25.1% cupric sulfate pentahydrate products and cupric 35.2 grams per liters according to a conventional method; Crystalline mother solution returns oxygen and presses the leaching process dosing.
Claims (1)
1. a thick tin is pressed except the direct acid oxygen of copper ashes and is leached treatment process, it is characterized in that, the method comprises the steps:
The thick tin of stanniferous 55～75%, the cupric 8～18% that (1) will produce when the thick tin of liquid state adds the sulphur copper removal is except copper ashes, be that 120～150 ℃, oxygen partial pressure are 0.15～0.25MPa, the acid of beginning is under the condition of 100～250 grams per liters in temperature, leached 4～6 hours, filter, obtain filtrate and filter residue that whole acid is 46～118 grams per liters
(2) be to carry out 6 hours thick tin of output of retailoring under 1200～1260 ℃ the condition in temperature with filter residue,
(3) according to a conventional method filtrate is concentrated crystallisation by cooling and produce the cupric sulfate pentahydrate product or carry out the electrolysis production electrolytic copper, liquid returns step (1) dosing after crystalline mother solution or the electrolysis.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074499A (en) * | 2013-01-31 | 2013-05-01 | 云南驰宏锌锗股份有限公司 | Method for producing high-quality copper sulfate through low-pressure oxygen leaching of copper slag |
| CN106521184A (en) * | 2016-11-04 | 2017-03-22 | 金少平 | Process for extracting copper sulfate through waste copper scraps |
| CN107034365A (en) * | 2017-06-08 | 2017-08-11 | 安徽省金鸿再生资源科技有限公司 | A kind of method of thick tin pyro-refining |
| CN108796237A (en) * | 2018-07-03 | 2018-11-13 | 云南锡业研究院有限公司 | A kind of wet treatment method of tin copper ashes |
| CN109971945A (en) * | 2019-04-25 | 2019-07-05 | 江西自立环保科技有限公司 | A kind for the treatment of process of coarse tin decoppered slag |
| CN110499521A (en) * | 2019-09-29 | 2019-11-26 | 湖南仁发材料科技有限公司 | A kind of method of copper electrolyte and copper removal scruff synergistic purification and processing |
| CN110551900A (en) * | 2019-09-29 | 2019-12-10 | 湖南仁发材料科技有限公司 | Combined treatment method for waste tin-plated copper scraps and copper electrolyte |
| CN111705216A (en) * | 2020-06-16 | 2020-09-25 | 云南锡业股份有限公司锡业分公司 | Treatment process of tin soldering electrolytic anode mud |
| CN114381608A (en) * | 2022-01-17 | 2022-04-22 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method of crude copper tin-removing slag |
| CN116103512A (en) * | 2022-12-30 | 2023-05-12 | 耒阳市焱鑫有色金属有限公司 | Pretreatment method for acid radical elution of tin mud acid leaching decoppering water |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074499A (en) * | 2013-01-31 | 2013-05-01 | 云南驰宏锌锗股份有限公司 | Method for producing high-quality copper sulfate through low-pressure oxygen leaching of copper slag |
| CN106521184A (en) * | 2016-11-04 | 2017-03-22 | 金少平 | Process for extracting copper sulfate through waste copper scraps |
| CN107034365A (en) * | 2017-06-08 | 2017-08-11 | 安徽省金鸿再生资源科技有限公司 | A kind of method of thick tin pyro-refining |
| CN107034365B (en) * | 2017-06-08 | 2019-03-15 | 安徽省金鸿再生资源科技有限公司 | A kind of method of thick tin pyro-refining |
| CN108796237A (en) * | 2018-07-03 | 2018-11-13 | 云南锡业研究院有限公司 | A kind of wet treatment method of tin copper ashes |
| CN109971945A (en) * | 2019-04-25 | 2019-07-05 | 江西自立环保科技有限公司 | A kind for the treatment of process of coarse tin decoppered slag |
| CN110499521A (en) * | 2019-09-29 | 2019-11-26 | 湖南仁发材料科技有限公司 | A kind of method of copper electrolyte and copper removal scruff synergistic purification and processing |
| CN110551900A (en) * | 2019-09-29 | 2019-12-10 | 湖南仁发材料科技有限公司 | Combined treatment method for waste tin-plated copper scraps and copper electrolyte |
| CN110499521B (en) * | 2019-09-29 | 2021-07-16 | 湖南仁发材料科技有限公司 | Method for cooperatively purifying and treating copper electrolyte and copper and tin slag |
| CN111705216A (en) * | 2020-06-16 | 2020-09-25 | 云南锡业股份有限公司锡业分公司 | Treatment process of tin soldering electrolytic anode mud |
| CN111705216B (en) * | 2020-06-16 | 2021-12-03 | 云南锡业股份有限公司锡业分公司 | Treatment process of tin soldering electrolytic anode mud |
| CN114381608A (en) * | 2022-01-17 | 2022-04-22 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method of crude copper tin-removing slag |
| CN116103512A (en) * | 2022-12-30 | 2023-05-12 | 耒阳市焱鑫有色金属有限公司 | Pretreatment method for acid radical elution of tin mud acid leaching decoppering water |
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Application publication date: 20130116 |