CN1333089C - Method for processing cobalt copper alloy - Google Patents
Method for processing cobalt copper alloy Download PDFInfo
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- CN1333089C CN1333089C CNB2005100620166A CN200510062016A CN1333089C CN 1333089 C CN1333089 C CN 1333089C CN B2005100620166 A CNB2005100620166 A CN B2005100620166A CN 200510062016 A CN200510062016 A CN 200510062016A CN 1333089 C CN1333089 C CN 1333089C
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Abstract
The present invention discloses a method for processing cobalt copper alloy, which comprises the steps that a mechanical activating process step, cobalt copper alloy is sent into a ball grinder to be ground coarsely firstly and is sent into a tube grinder to be ground finely, and after ground for two times, cobalt copper alloy powders have large internal energy and surface energy and a high specific surface area and further have high reaction activity; a leaching process step, slurry of the cobalt copper alloy powders is filled into a reaction leaching tank, water and Hydrochloric acid are added in a definite proportions, the mixture is heated and stirred under the conditions of catalysis and oxidation to leach 90% to 99% of valent metals, namely cobalt and copper, and make the valent metals enter solution; a magnetic separating process step, a weak magnetic separator is utilized to separate a small amount of unreacted residual cobalt copper alloy in leach slurry from the slurry, the slurry after the magnetic separation is filtered to separate solids from liquid, and cobalt-rich and copper-rich solution can be obtained. The present invention has the advantages of short technical process, low production cost, high leaching rate of cobalt and copper, high extraction rate, etc.
Description
Technical field
The present invention relates to a kind of method of handling cobalt-copper alloy, particularly a kind of method with the wet processing cobalt-copper alloy.
Background technology
Cobalt-copper alloy is the important source material of producing cobalt metal and various cobalt products, is commonly called as cobalt white metal or cobalt red alloy or cobalt AB alloy, mainly originates from Africa.Cobalt-copper alloy makes by electric furnace reduction melting cupric oxide cobalt concentrate and the copper slag that contains cobalt, generally contains cobalt: 10%-40%, copper: 10%-50%, iron: 5%-50%, nickel: 0.1%-5%, manganese: 0.1%-5%.This alloy raw material intractability is bigger, and subject matter is that the yield of cobalt, copper is low, cost is high, technical process is long.
The method of handling cobalt-copper alloy at present mainly contains:
1, electro-dissolving: in electrolyzer, be anode, in sulfuric acid or hydrochloric acid system, make cobalt, copper enter solution from the anode dissolving by electrolysis with the cobalt-copper alloy raw material, manganese, iron, nickel also together dissolving enter solution.This method current efficiency is lower, power consumption is higher, and the rate of recovery of cobalt is lower.
2, sulfuration lixiviation process: the cobalt-copper alloy raw material is added sulphur or sulfide (as sulfurous iron ore) sulfuration under 1300 ℃ of-1400 ℃ of temperature, after the oxidation blowing deironing, obtain Co-Cu ice sulfonium and leach the solution that obtains containing cobalt, copper through high pressure.This method production capacity is big, technical process is long, energy consumption is high, and the total recovery of cobalt, copper is lower.
3, High Temperature High Pressure lixiviation process: leach by one section normal pressure and one section High Temperature High Pressure leaching with sulfuric acid or hydrochloric acid, make cobalt, copper leaching in the cobalt-copper alloy enter solution.This method technical process is long, equipment is complicated, must solve the anticorrosion problem of equipment under high temperature, the condition of high voltage.
4, chlorine lixiviation process: this method is to carry out in airtight reactor, behind cobalt-copper alloy and hydrochloric acid adding reactor, feeds chlorine and carries out oxidation dissolution.The leaching yield of this method cobalt, copper, iron higher (mining and metallurgy, 1997, Vol6 (1): 67-69), but equipment complexity, equipment anticorrosion and environmental requirement height.
5, direct pickling process: leach with sulfuric acid, hydrochloric acid or nitric acid or two kinds of composition mixing acid wherein.This method is under normal pressure, and speed of response is slow, and leaching process efficient is not high, and technical process is long, the production cost height.
In addition, above-mentioned the whole bag of tricks enters leach liquor because a large amount of iron also leaches simultaneously, and the iron removal of postorder will cause the loss of cobalt, copper, directly influence the rate of recovery of cobalt, copper.
Summary of the invention
For overcoming existing treatment process above shortcomings, the invention provides that a kind of technical process is short, production cost is low, cobalt copper leaching rate and the high a kind of method of handling cobalt-copper alloy of casting yield.The technical solution adopted for the present invention to solve the technical problems is that it may further comprise the steps:
(1), mechanical activation operation: at first cobalt-copper alloy is sent into ball mill or Raymond mill is roughly ground, and then send into tuber grinder or vibrations mill or mechanical stirring mill and carry out fine grinding, by making the cobalt-copper alloy powder have high interior energy, surface energy and high specific surface area behind two sections mills, and then make the cobalt-copper alloy powder have high reactive behavior;
(2), leach operation: will add reactive tank through the cobalt-copper alloy powder or the slip of mechanical activation; By the solvent and solute weight ratio 3 in the reactive tank: 1-12: 1 adds entry and adds hydrochloric acid by the 75%-150% of theoretical value; Be not more than 150g/L by catalyst concn again and add catalyzer, described catalyzer is to contain at least a in the inorganic salt of haloid element; The oxygenant that adds the 0.2-2.0 cubic meter again by every cubic metre of slip under heating, agitation condition, makes cobalt, copper valuable metal 90%-99% leaching in the cobalt-copper alloy enter solution;
(3), magnetic separation separation circuit: utilize the cobalt-copper alloy magnetic properties different with leached mud, to leach by the low intensity magnetic separation machine that unreacted small portion of residual cobalt-copper alloy separates with slip in the slip, slip after the magnetic separation filters by B, makes solid-liquid separation, can obtain being rich in the solution of cobalt, copper.
The median size of the cobalt-copper alloy powder of process mechanical activation is between 10 μ m-150 μ m.
The pH value of solution value of described leaching operation reaction end is controlled between the 2.0-4.5.
The temperature of reaction that leaches operation is controlled between 65 ℃-95 ℃, and the reaction times is controlled between the 200min-900min.
Described oxygenant is at least a in air, the oxygen.
The small portion of residual cobalt-copper alloy that magneticly elects turns back to the mechanical activation operation or leaches operation.
The inorganic salt of described haloid element are Repone K, sodium-chlor, iron(ic) chloride, iron protochloride, cupric chloride, ammonium chloride, sodium chlorate, Sodium Fluoride, Neutral ammonium fluoride, ammonium bifluoride
After adopting aforesaid method, following characteristics are arranged: the one, technical process is short, under condition of normal pressure, can make the leaching yield of cobalt in the cobalt-copper alloy, copper reach 90%-99%, and the iron rule in the alloy is stayed in the leached mud with the form of ferric oxide or pyrrhosiderite; The 2nd, simple to operate, be easy to control; The 3rd, it is very fast to leach speed of response, and it is higher to leach operating efficiency; The 4th, the leaching yield height of cobalt and copper, the casting yield height of cobalt and copper; Five reduced investments, production cost is lower.
Embodiment
Below in conjunction with specific embodiments main processes of the present invention is sketched: it may further comprise the steps:
(1), mechanical activation operation: at first cobalt-copper alloy is sent into ball mill or Raymond mill is roughly ground, and then send into tuber grinder or vibrations mill or mechanical stirring mill and carry out fine grinding, by making the cobalt-copper alloy powder have high interior energy, surface energy and high specific surface area behind two sections mills, and then make the cobalt-copper alloy powder have high reactive behavior; The median size of the cobalt-copper alloy powder of process mechanical activation is between 10 μ m-150 μ m.
(2), leach operation: at first will add reactive tank through the cobalt-copper alloy powder or the slip of mechanical activation, then by the interior solvent and solute weight ratio 3 of reactive tank: 1-12: 1 adds entry and by the 75%-150% adding hydrochloric acid of theoretical amount; The amount that is not more than 150g/L by catalyst concn adds catalyzer again, and described catalyzer is to contain at least a in the inorganic salt of haloid element, also can be several combinations; Then add oxygenant again, described oxygenant is at least a in air, the oxygen, and the oxygenant add-on is controlled at every cubic metre of slip 0.2-2.0 cubic meter; And stir, the rotating speed of stirring rake is 80-350 rev/min; With steam or electricity slip is heated between 65 ℃-95 ℃; Reaction times is controlled between the 300min-900min; By the relative quantity or the adding neutralizing agent of control reactive tank internal reaction material, the pH value of control reaction end, the pH value is controlled between the 2.0-4.5, makes cobalt, copper valuable metal 90%-99% leaching in the cobalt-copper alloy enter solution.
On the catalyzed oxidation leaching process, cobalt-copper alloy and hydrochloric acid can also can add in batches in disposable adding; The degree of the add-on of catalyzer and the mechanical activation of cobalt-copper alloy is relevant with the ionic strength of leach liquor; When the degree of mechanical activation is good, can add less or not add, excessive catalyzer can cause the passivation of alloy; The amount of blasting of oxygenant air or oxygen can be different in initial stage, mid-term and the later stage of reaction, oxygenant should be in reactive tank homodisperse, guarantee and fully the contacting of feed liquid.
(3), magnetic separation separation circuit: magnetic separation is the important means of simplifying leaching operation, quickening leaching velocity and guaranteeing cobalt, copper casting yield; Cobalt-copper alloy has stronger ferromegnetism, and leached mud does not have, and utilizes cobalt-copper alloy different with the magnetic properties of leached mud, will leach by the low intensity magnetic separation machine that unreacted small portion of residual cobalt-copper alloy separates with slip in the slip; The cobalt-copper alloy that magneticly elects is back to the mechanical activation operation or leaches operation; Filter by B through the slip after the magnetic separation, make solid-liquid separation, can obtain being rich in the solution of cobalt, copper.A series of problems that the chemical equilibrium of reactive tank internal reaction material causes have been solved well by magnetic separation.Because, the one, the cobalt-copper alloy powder in the reactive tank and hydrochloric acid add-on are difficult to accomplish just in time to add by the dosage of equivalent chemical reaction, even accomplish or near equivalent, speed is also very slow when reacting near terminal point; The 2nd, for fast reaction speed, one of them that must make cobalt-copper alloy or hydrochloric acid in the reaction leaching vat is excessive; The 3rd, in order to guarantee the leaching yield of cobalt, copper, must add excessive hydrochloric acid, and excessive hydrochloric acid will increase difficulty to the control of reaction process pH value, the consumption of material also will increase.
The inorganic salt of described haloid element are Repone K, sodium-chlor, iron(ic) chloride, iron protochloride, cupric chloride, ammonium chloride, sodium chlorate, Sodium Fluoride, Neutral ammonium fluoride, ammonium bifluoride.
Enter leach liquor in order to prevent that a large amount of iron from also leaching simultaneously, add-on that can be by catalyzer, oxygenant and hydrochloric acid and temperature of reaction and reaction times are controlled the leaching of iron in the cobalt-copper alloy; After adopting aforesaid method, the leaching yield of iron is less than 1.0%, and the content of iron can be controlled in below the 0.5g/L in the leach liquor, the minimum 5PPm that reaches.
Be that the cobalt-copper alloy of cobalt 28.7%, copper 26.3%, iron 23.5%, nickel 1.08%, manganese 0.89% is illustrated with major ingredient below.
Embodiment one gets cobalt-copper alloy 1000 grams and put into the ball mill mill 90 minutes, and then shakes mill 120 minutes, and median size is 47 microns.Weigh this alloy 80 grams, ammonium chloride 80 grams, iron(ic) chloride 20 grams, 133 milliliters of 36% hydrochloric acid add 500 milliliters in water, heat up to be heated to 87 degree, bubbling air (add-on is controlled at every cubic metre of slip 0.2-2.0 cubic meter), reaction is 8 hours under agitation condition, and reaction end pH value is 3.5.Then slip is carried out magnetic separation, filtration.Magneticly elect unreacted remaining cobalt-copper alloy 2.6 grams, the leach liquor that obtains contains cobalt 26.9 grams per liters, copper 24.8 grams per liters, iron 0.06 grams per liter.Leached mud contains cobalt 0.42 gram, copper 0.30 gram.The leaching yield of cobalt is 94.3%, and the leaching yield of copper is 95.2%.The casting yield of cobalt is 98.0%, and the casting yield of copper is 98.3%.
Embodiment two gets cobalt-copper alloy 1000 grams and put into the ball mill mill 90 minutes, and then shakes mill 120 minutes, and median size is 47 microns.Weigh this alloy 80 grams, ammonium chloride 50 grams, Sodium Fluoride 30 grams, 133 milliliters of 36% hydrochloric acid add 500 milliliters in water, heat up to be heated to 87 degree, bubbling air (add-on is controlled at every cubic metre of slip 0.2-2.0 cubic meter), reaction is 8 hours under agitation condition, and reaction end pH value is 3.5.Then slip is carried out magnetic separation, filtration.Magneticly elect unreacted remaining cobalt-copper alloy 2.1 grams, the leach liquor that obtains contains cobalt 32.8 grams per liters, copper 27.6 grams per liters, iron 0.08 grams per liter.Leached mud contains cobalt 0.31 gram, copper 0.33 gram.The leaching yield of cobalt is 95.8%, and the leaching yield of copper is 95.5%.The casting yield of cobalt is 98.4%, and the casting yield of copper is 98.2%.
Embodiment three gets cobalt-copper alloy 1000 grams and put into the ball mill mill 90 minutes, and then shakes mill 120 minutes, and median size is 47 microns.Weigh this alloy 160 grams, ammonium chloride 50 grams, Sodium Fluoride 30 grams, iron(ic) chloride 20 grams, 266 milliliters of 36% hydrochloric acid, add 500 milliliters in water, intensification is heated to 87 degree, bubbling air (add-on is controlled at every cubic metre of slip 0.2-2.0 cubic meter), and reaction is after 6.5 hours under agitation condition, slowly sodium hydroxide solution to the pH value of adding 5% is 4.0, continues reaction 45 minutes.Then slip is carried out magnetic separation, filtration.Magneticly elect unreacted remaining cobalt-copper alloy 3.5 grams, the leach liquor that obtains contains cobalt 57.2 grams per liters, copper 50.0 grams per liters, iron 0.005 grams per liter.Leached mud contains cobalt 0.39 gram, copper 0.77 gram.The leaching yield of cobalt is 96.6%, and the leaching yield of copper is 95.6%.The casting yield of cobalt is 98.9%, and the casting yield of copper is 97.3%.
Embodiment four cobalt-copper alloys 1000 grams were put into the ball mill mill 90 minutes, and then shook mill 120 minutes, and median size is 47 microns.Weigh these alloy 135 grams and magneticly elect and leach unreacted cobalt-copper alloy 25 grams in the slip, ammonium chloride 50 grams, Sodium Fluoride 30 grams, iron(ic) chloride 20 grams, 266 milliliters of 36% hydrochloric acid, add 500 milliliters in water, intensification is heated to 87 degree, bubbling air (add-on is controlled at every cubic metre of slip 0.2-2.0 cubic meter), and reaction is 6.5 hours under agitation condition, slowly adding ammonia pH value is 4.0, continues reaction 45 minutes.Then slip is carried out magnetic separation, filtration.Magneticly elect unreacted remaining cobalt-copper alloy 4.2 grams, the leach liquor that obtains contains cobalt 54.2 grams per liters, copper 51.3 grams per liters, iron 0.006 grams per liter.Leached mud contains cobalt 0.15 gram, copper 0.83 gram.The leaching yield of cobalt is 96.7%, and the leaching yield of copper is 94.4%.The casting yield of cobalt is 99.2%, and the casting yield of copper is 97.5%.
Claims (7)
1, a kind of method of handling cobalt-copper alloy, it is characterized in that: it may further comprise the steps:
(1), mechanical activation operation: at first cobalt-copper alloy is sent into ball mill or Raymond mill is roughly ground, and then send into tuber grinder or vibrations mill or mechanical stirring mill and carry out fine grinding, by making the cobalt-copper alloy powder have high interior energy and surface energy and high specific surface area behind two sections mills, and then make the cobalt-copper alloy powder have high reactive behavior;
(2), leach operation: will add reactive tank through the cobalt-copper alloy powder or the slip of mechanical activation; By the solvent and solute weight ratio 3 in the reactive tank: 1-12: 1 adds entry and adds hydrochloric acid by the 75%-150% of theoretical value; Be not more than 150g/L by catalyst concn again and add catalyzer, described catalyzer is to contain at least a in the inorganic salt of haloid element; The oxygenant that adds the 0.2-2.0 cubic meter again by every cubic metre of slip under heating, agitation condition, makes cobalt, copper valuable metal 90%-99% leaching in the cobalt-copper alloy enter solution;
(3), magnetic separation separation circuit: utilize the cobalt-copper alloy magnetic properties different with leached mud, to leach by the low intensity magnetic separation machine that unreacted small portion of residual cobalt-copper alloy separates with slip in the slip, slip after the magnetic separation filters by B, makes solid-liquid separation, can obtain being rich in the solution of cobalt, copper.
2, a kind of method of handling cobalt-copper alloy according to claim 1 is characterized in that: the median size of the cobalt-copper alloy powder of process mechanical activation is between 10 μ m-150 μ m.
3, a kind of method of handling cobalt-copper alloy according to claim 1, it is characterized in that: the pH value of solution value of described leaching operation reaction end is controlled between the 2.0-4.5.
4, a kind of method of handling cobalt-copper alloy according to claim 1 is characterized in that: the temperature of reaction that leaches operation is controlled between 65 ℃-95 ℃, and the reaction times is controlled between the 200min-900min.
5, a kind of method of handling cobalt-copper alloy according to claim 1 is characterized in that: described oxygenant is at least a in air, the oxygen.
6, a kind of method of handling cobalt-copper alloy according to claim 1 is characterized in that: the small portion of residual cobalt-copper alloy that magneticly elects turns back to the mechanical activation operation or leaches operation.
7, a kind of method of handling cobalt-copper alloy according to claim 1, it is characterized in that: the inorganic salt of described haloid element are Repone K, sodium-chlor, iron(ic) chloride, iron protochloride, cupric chloride, ammonium chloride, sodium chlorate, Sodium Fluoride, Neutral ammonium fluoride, ammonium bifluoride.
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| CN101818246B (en) * | 2010-05-11 | 2012-05-23 | 南通新玮镍钴科技发展有限公司 | Technology for leaching cobalt-copper white alloy |
| CN102392126A (en) * | 2011-11-17 | 2012-03-28 | 森松(江苏)海油工程装备有限公司 | Activating acid leaching method for extracting vanadium from bone coal |
| CN103128288A (en) * | 2011-11-22 | 2013-06-05 | 元磁新型材料(苏州)有限公司 | Metal crystal powder and production method and production device thereof |
| CN105755283B (en) * | 2016-03-08 | 2017-09-12 | 江西理工大学 | The method of valuable metal in villaumite Selectively leaching lateritic nickel ore |
| CN106040409A (en) * | 2016-08-24 | 2016-10-26 | 孙召华 | Ore-dressing system and ore-dressing technology for reducing content of sulphur in iron ore concentrate and for sorting cobalt concentrate |
| CN109652651A (en) * | 2017-10-10 | 2019-04-19 | 中国石油化工股份有限公司 | The method of the useless activation of cobalt molybdenum base hydrotreating catalyst Call Provision and molybdenum |
| CN109897968A (en) * | 2019-04-21 | 2019-06-18 | 湖南金源新材料股份有限公司 | A method of leaching rate is improved using ultra-fine grinding mill processing lithium battery reworked material |
| CN110629223B (en) * | 2019-10-15 | 2021-07-06 | 上海第二工业大学 | Deplating method for metal coating on surface of waste ABS electroplated part |
| EP4200452A1 (en) | 2020-08-18 | 2023-06-28 | Enviro Metals, LLC | Metal refinement |
| CN112609090B (en) * | 2020-11-19 | 2022-10-14 | 中国恩菲工程技术有限公司 | Separation method of copper-cobalt oxide ore |
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| JPS5489904A (en) * | 1977-12-27 | 1979-07-17 | Sumitomo Metal Mining Co | Separating of valuable metal from rare earth element containing alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5489904A (en) * | 1977-12-27 | 1979-07-17 | Sumitomo Metal Mining Co | Separating of valuable metal from rare earth element containing alloy |
Non-Patent Citations (1)
| Title |
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| 矿冶 王含渊，江培海，张寅生，黄忠淼，67.69，钴白合金湿法冶金工艺研究 1997 * |
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