CN101787434A - Method for recovering iron and tin-lead-zinc from magnetic separation waste residue by rotary kiln through deoxygenation, chloridization and oxidation - Google Patents
Method for recovering iron and tin-lead-zinc from magnetic separation waste residue by rotary kiln through deoxygenation, chloridization and oxidation Download PDFInfo
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- CN101787434A CN101787434A CN201010117493A CN201010117493A CN101787434A CN 101787434 A CN101787434 A CN 101787434A CN 201010117493 A CN201010117493 A CN 201010117493A CN 201010117493 A CN201010117493 A CN 201010117493A CN 101787434 A CN101787434 A CN 101787434A
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Abstract
The invention relates to a method for recovering iron and tin-lead-zinc from magnetic separation waste residue by a rotary kiln through deoxygenation, chloridization and oxidation, comprising the following steps of: mixing coke powder accounting for 5 to 6% of the weight of the waste by dry weight percent with the magnetic separation waste residue for uniformly stirring; adding calcium chloride solution for uniformly stirring; preparing balling by a pelletizer; drying balling materials by a grate and delivering the materials to the rotary kiln for chloridizing roasting with high temperature; inhaling smoke of the rotary kiln to a dry type dust collection system for recovering dust solid volatile by an exhaust fan to obtain a mixture of the tin-lead-zinc and the iron; and discharging baked dregs from a kiln head to form qualified iron ore concentrate, wherein the kiln discharge temperature of the smoke is 210 to 250 DEG C; and the temperature of the smoke of the dust collection device is 95 to 110 DEG C. The invention can stably process the high-iron low-tin magnetic waste containing the tin as low as 0.1% and the arsenic as high as 0.6 to 1.5%, the qualified iron ore concentrate and tin ore containing 3 to 5% of tin are produced, and lead-zinc-copper is separated and recovered from the tin ore. Compared with the traditional high-temperature chloridization-wet dust collection process, the invention has the same evaporation rate of the tin-lead-zinc and the arsenic, short process, no corrosion and long service life of the device and reduces thet production cost by 20 to 50%.
Description
Technical field the invention belongs to a kind of rotary kiln reduction chlorination and adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation.Also comprise the recovery of non-ferrous metals such as copper arsenic.
Background technology often produces the symbiotic difficultly separable tin middling of a lot of iron tin, magnetic tailing reluctant materials such as (claiming magnetic separation waste residue again) in many tin ore ore dressings.Magnetic separation waste residue (limonite) particularly, surmise thin, non-ferrous metal content such as tin are low, iron level is up to 45%-55%, but because foreign matter content height such as its arsenic, do not meet the requirement of blast furnace ironmaking and is used as unserviceable solid waste by people for a long time, abandon in a large number before and after col and the factory building, raise with wind arbitrarily in dry date at air-dry thing, fill the air in air contaminate environment.Though people find out a lot of ways and remove impurity such as arsenic satisfying the requirement of ironmaking, too high because of cost, process is complicated and drop one after another.
Processing for the higher difficultly separable tin middling of stanniferous, once disclosed authorization in 1992 and number be the Chinese patent of CN1018932B " high-temp chlorination method of difficultly separable tin middling ", and international ore dressing in 1984 and extraction are controlled the paper in the golden proceeding (extracting metallurgical part), " high temperature chlorination roastings of the low many metalliferous materials of tin high ferro ".The principle of these two kinds of methods all is chloridizing volatilization, all is the non-ferrous metals such as tin copper-lead zinc arsenic in the material to be become volatilizable muriate earlier enter flue dust, reclaims with wet dust collection equipment again, and iron rule becomes iron ore concentrate with the form of roasting slag.Both differences only are concrete steps and interpolation chlorizating agent, go back the kind of raw coal and quantitatively variant.In addition, above-mentioned patented method also will bake ball and sinter the chou piece into, make the intensity of pelletizing meet the requirement of blast furnace ironmaking more.
Owing to contain a large amount of chlorine in the flue dust of chloridizing volatilization, generally believe the corrosion of equipment too greatly, be not suitable for reclaiming and can only handling with the wet dust collection method with dry dust collection.And the equipment of wet dust collection is many, and treating processes is tediously long, and production cost is higher, and dust collection effect also not necessarily is better than dry dust collection.
For the magneticore-dressing plant's high-iron and low-tin waste residue that abandons in a large number, its tin grade is mostly below 1%, and what have is low to moderate 0.3%, and the content of arsenic is up to 0.5-1%.Though iron level is up to 45-55%, but still do not meet the iron work requirement, even foreign matter contents such as arsenic meet the requirements, be reduced to below the 0.07-0.15%, non-ferrous metals such as the tin of high value are not also counted valency, under the low price condition of iron ore concentrate, remaining with this magnetic separation waste residue of existing technical finesse loses more than gain, this solid waste is turned waste into wealth, must improve prior art, reduce cost significantly, particularly overcome the equipment corrosion problem in the process of gathering dust, just can make the realization of this target become possibility.
Summary of the invention purpose of the present invention is exactly can't the effective recycling problem at magnetic separation waste residue, propose that a kind of equipment corrosion is little, production efficiency is high, recovery arsenic simultaneously can volatilize, and non-ferrous metal such as tin, lead and zinc copper, the rotary kiln of the qualified iron ore concentrate of output reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, solves the deficiencies in the prior art with this.
This rotary kiln reduction chlorination that the present invention proposes adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, it is characterized in that it has the following steps:
(1) in magnetic separation waste residue, mix by dry weight basis, account for waste residue weight 5-6% coke powder and mix thoroughly;
(2) adding calcium chloride water stirs;
(3) will go up step gained material and make pelletizing with pelletizer;
(4) the pelletizing material is sent into rotary kiln after with the drying grate drying and is carried out high temperature chlorination roasting;
(5) flue gas of rotary kiln sucks dry dust collection system recoveries dust solid volatile matter with vacuum fan, gets the mixture byproduct of tin, lead and zinc and arsenic;
(6) the roasting slag of rotary kiln is from the qualified iron ore concentrate of kiln hood discharge becoming.
The calcium chloride add-on in (2) step should be calculated by the required chlorizating agent theoretical amount of the whole chlorinations of metals such as tin, lead and zinc, and generally the 2-2.5 with theoretical amount extraordinarily goes into.
The ball operation equipment used of making in (3) step is a bowl granulator, and the pelletizing material of making is introduced into sieve apparatus, and screen underflow returns pelletizer pelletizing again, and screen overflow then enters the drying grate drying, to increase ultimate compression strength.
The control kiln temperature is divided into successively from kiln tail to kiln hood: the preheating zone temperature is that 230-800 ℃, zone of reduction temperature are that 800-1100 ℃, chloridizing volatilization band temperature are that 1100-1300 ℃, strong zone of oxidation temperature are that 600-1100 ℃ and cooling zone temperature are 400-600 ℃.
Flue gas kiln discharge temperature is controlled at 210-250 ℃, and the facility flue-gas temperature of gathering dust is 95-110 ℃.
The gained mix products that gathers dust is the mixed powder that contains tin, lead and zinc and arsenic, separates non-ferrous metals such as tin, lead and zinc with existing smelting process.
The roasting slag of discharging from kiln hood cools off through the rotation cooling cylinder.The cooling cylinder inner ventilation, the drum outer wall spraying cooling water.
Pelletizing enters into from the kiln hood discharge from the tail end of kiln body, is experiencing successive reduction-chlorination and oxidizing reaction.Non-ferrous metals such as tin, lead and zinc arsenic are chlorinated into chloride-sublimation, enter dust collecting system with air-flow.The most elder generations of arsenic are reduced into lower valency from high valence state and enter strong oxidation panel, enter flue gas again.The following chemical reaction takes place in this process:
As
2O
5+2CO→As
2O
3↑+CO
2↑
SnO
2+CO→SnO+CO
2↑
SnO+2CaCl
2→SnCl
4↑+CaO
SnCl
4+O
2→SnO
2+Cl
2↑
Pb
2O
3+CO+2CaCl
2→2PbCl
2↑+CO
2↑+2CaO
ZnO+CO+CaCl
2→ZnCl
2↑+CO
2↑+CaO
4AsFeO
4+2C→2As
2O
3↑+2Fe
2O
3+2CO
2↑
The reaction of carrying out in the rotary kiln also more than these, but main be above-mentioned several.After so reduction-chloride-oxidation reacted, variation had all taken place in the form and the position of non-ferrous metals such as the arsenic in the magnetic separation waste residue, tin, lead and zinc, has been divided into roasting slag and flue dust.Iron etc. mainly concentrate on and bake slag, and non-ferrous metals such as arsenic and tin, lead and zinc are then transferred in the flue dust.The chlorine that the muriate of roasting process generates is met water and is hydrochloric acid, will cause heavy corrosion to the metal dust collection device.
The present invention is directed to this problem, strict control flue dust temperature has been avoided serious equipment corrosion, and rotary kiln and dry-type dust collection system all are able to normal operation.
Processing method of the present invention can stably be handled stanniferous and be low to moderate 0.1%, contains the high-iron and low-tin magnetic separation waste residue of arsenic up to 0.6-1.5%, and the medium tin ore of qualified iron ore concentrate of output and stanniferous 3-5%, plumbous zinc-copper equal in the medium tin ore Separation and Recovery again.Than existing high-temp chlorination-wet dust collection technology, the evaporation rate index of tin, lead and zinc and arsenic is suitable, and operation is short, service life of equipment is long but gather dust, and production cost hangs down 20-50%.
Appended drawings is a process flow sheet of the present invention.
Embodiment adopts the combustion unit of inventor ZL2008100584074 patent and the rotary kiln that this patent document is addressed to handle 400 ton per days (dry weight) magnetic separation waste residue as shown in the figure.Method steps is: the coke powder that mixes 5-6% in magnetic separation waste residue is mixed thoroughly, deliver in the screw mixer with rotary conveyor and to mix thoroughly with calcium chloride water, calcium chloride add-on with dry weight basis is the 4-6% of magnetic separation waste residue dry weight, the preparation of calcium chloride water and prior art, basic identical as the Chinese patent " high-temp chlorination method of difficultly separable tin middling " of above-mentioned CN1018932B.Admix the material of calcium chloride water and send into pan-type pelletizer, send into roller type sieving machine after causing the pelletizing of diameter 0.8-2cm, screen underflow returns granulating disc pelletizing again, and the pelletizing on the sieve enters promptly to be sent into rotary kiln after the drying grate drying and carry out high temperature chlorination roasting.Magnetic separation waste residue is that streamline is worked continuously from mixing powdered carbon to entering rotary kiln.
This technology is controlled to be in the temperature of the φ 3 * 50m of Gejiu enterprise rotary kiln: from kiln tail end mouth to 20 meter section is the drying and preheating section, and temperature is 230-800 ℃; 20-30 rice section is a zone of reduction, and temperature is 800-1100 ℃; 30-40 rice section is the chloridizing volatilization band, and temperature is 1100-1300 ℃; 40-45 rice Duan Weiqiang zone of oxidation, temperature is 600-1100 ℃; 45-50 rice section is a cooling zone, and temperature is 400-600 ℃.The flue-gas temperature of rotary kiln (kiln discharge temperature) is controlled at 210-250 ℃; The facility that gathers dust is controlled at 95-110 ℃, and the rotating speed of rotary kiln is 0.5-0.9 rev/min.
Dry-type dust collection system is commercially available chemical fabric bag collector.
Be 18 days working cycle, 6400 tons of magnetic separation waste residue treatment capacities, material composition: Fe 52%, Sn 0.52%, Pb 0.86%, Zn 0.6%, As 0.83%.After this art breading, must bake 5120 tons of slags, 570 tons of flue dust, all the other are crystal water volatilization and mechanical loss in the slag.
The gained technical indicator is as follows:
Flue dust composition: (%)
Fe?18.36、Sn?4.73、Pb?8.59、Zn?3.82、As?8.58、
Roasting slag (iron ore concentrate) composition: (%)
Fe?60.56 Sn?0.11 Pb?0.106 Zn?0.29 As?0.093
The evaporation rate of each element in the magnetic separation waste residue: (%)
Sn?82 Pb?90 Zn?57 As?92。
And the 5000 tons of magnetic separation waste residue that used the same method with device processes, composition becomes: when Fe 53%, Sn 0.1%, Pb 1.2%, Zn 0.5%, As1.5%j.Get 4008 tons of roasting slags, 451 tons of flue dust, all the other are volatilization of magnetic separation waste residue crystal water and mechanical loss.
The gained technical indicator is as follows:
Flue dust composition: (%)
Fe?19.54、Sn?1.01、Pb?11.79、Zn?3.98、As?15.39、
Roasting slag (iron ore concentrate) composition: (%)
Fe?62.56 Sn?0.06 Pb?0.156 Zn?0.49 As?0.102
The evaporation rate of each element in the magnetic separation waste residue: (%)
Sn?91 Pb?88.6 Zn?71.8 As?92.5。
The evaporation rate of each element points to the rate of transform in the flue dust in the above-mentioned magnetic separation waste residue, does not count the part in the mechanical loss.What all the other indexs of roasting slag (iron ore concentrate) met iron work fully goes into the stove requirement, all sells the on-site iron and steel enterprise with the applicant.Before and after after the two batches of flue dust products mix, stanniferous greater than 3% medium tin ore, the sale of all being valuated.Economic benefit is very considerable.
Aforesaid method is many half a year in the trial run of Yunnan enterprise, and dry-type dust collection system does not still have any damaged, so far in normal use, estimates that work-ing life is more than 3 years.
Claims (7)
1. rotary kiln reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, it is characterized in that it has the following steps:
(1) in magnetic separation waste residue, mix by dry weight basis, account for waste residue weight 5-6% coke powder and mix thoroughly;
(2) adding calcium chloride water stirs;
(3) will go up step gained material and make pelletizing with pelletizer;
(4) the pelletizing material is sent into rotary kiln after with the drying grate drying and is carried out high temperature chlorination roasting;
(5) flue gas of rotary kiln sucks dry dust collection system recoveries dust solid volatile matter with vacuum fan, gets the mixture byproduct of tin, lead and zinc and arsenic;
(6) the roasting slag of rotary kiln is from the qualified iron ore concentrate of kiln hood discharge becoming.
2. rotary kiln according to claim 1 reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, and the calcium chloride add-on that it is characterized in that for (2) step is doubly calculated by the 2-2.5 of the required chlorizating agent theoretical amount of the whole chlorinations of metals such as tin, lead and zinc.
3. rotary kiln according to claim 1 and 2 reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, it is characterized in that the calcium chloride add-on is that the 4-6% of magnetic separation waste residue dry weight adds.
4. rotary kiln according to claim 1 reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, the ball operation equipment used of making that it is characterized in that for (3) step is a bowl granulator, the pelletizing material of making is introduced into sieve apparatus, screen underflow returns pelletizer pelletizing again, screen overflow then enters the drying grate drying, to increase ultimate compression strength.
5. rotary kiln according to claim 1 reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, it is characterized in that being divided into successively from kiln tail to kiln hood: the preheating zone temperature is that 230-800 ℃, zone of reduction temperature are that 800-1100 ℃, chloridizing volatilization band temperature are that 1100-1300 ℃, strong zone of oxidation temperature are that 600-1100 ℃ and cooling zone temperature are 400-600 ℃.
6. rotary kiln according to claim 1 reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, and it is characterized in that controlling flue gas kiln discharge temperature is 210-250 ℃, and the facility flue-gas temperature of gathering dust is 95-110 ℃.
7. rotary kiln according to claim 1 reduction chlorination adds the method that iron and tin, lead and zinc in the magnetic separation waste residue are reclaimed in oxidation, and the gained mix products that it is characterized in that gathering dust separates the tin, lead and zinc non-ferrous metal with existing smelting process.
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| CN102534188A (en) * | 2012-01-20 | 2012-07-04 | 个旧市富祥工贸有限责任公司 | Method for producing iron pellet with sulfur acid residue containing large contents of impurities and enriching valuable metal |
| CN102560088A (en) * | 2012-01-20 | 2012-07-11 | 个旧市富祥工贸有限责任公司 | Composite chlorinating metallurgy method for full-value utilization of complex poor tin middling ore |
| CN102925673A (en) * | 2012-10-29 | 2013-02-13 | 云南锡业集团有限责任公司研究设计院 | Method for treating high-iron low-tin ores |
| CN104164572A (en) * | 2014-08-25 | 2014-11-26 | 北京矿冶研究总院 | Method for recovering valuable metals in tailings |
| CN107151741A (en) * | 2017-06-06 | 2017-09-12 | 江苏省冶金设计院有限公司 | A kind of system and method for handling lead and zinc smelting dreg |
| CN107201442A (en) * | 2017-06-06 | 2017-09-26 | 江苏省冶金设计院有限公司 | A kind of system and method for handling zinc leaching residue |
| CN107739817A (en) * | 2017-10-10 | 2018-02-27 | 北京矿冶研究总院 | Method for calcified chlorination and volatilization comprehensive resource utilization of jarosite slag |
| CN108486384A (en) * | 2018-03-16 | 2018-09-04 | 湖南腾驰环保科技有限公司 | The recovery process of low-grade stanniferous bismuth tungsten slag |
| CN109338111A (en) * | 2018-11-27 | 2019-02-15 | 贵州省兴安环保科技有限公司 | A method of from recycling valuable metal in material containing zinc-tin |
| CN112591831A (en) * | 2020-12-04 | 2021-04-02 | 兰州有色冶金设计研究院有限公司 | Harmless treatment method for strongly acidic mine tailings |
| CN112877537A (en) * | 2021-01-13 | 2021-06-01 | 何良东 | Method and system for high-temperature chlorination treatment of solid waste |
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| CN101280917A (en) * | 2008-05-13 | 2008-10-08 | 吕伟鹏 | Coal gas, coal fines and oxygen-enriched mixed combustion method and device |
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Patent Citations (1)
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| CN101280917A (en) * | 2008-05-13 | 2008-10-08 | 吕伟鹏 | Coal gas, coal fines and oxygen-enriched mixed combustion method and device |
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| CN102534188A (en) * | 2012-01-20 | 2012-07-04 | 个旧市富祥工贸有限责任公司 | Method for producing iron pellet with sulfur acid residue containing large contents of impurities and enriching valuable metal |
| CN102560088A (en) * | 2012-01-20 | 2012-07-11 | 个旧市富祥工贸有限责任公司 | Composite chlorinating metallurgy method for full-value utilization of complex poor tin middling ore |
| CN102560088B (en) * | 2012-01-20 | 2013-10-02 | 个旧市富祥工贸有限责任公司 | Composite chlorinating metallurgy method for full-value utilization of complex poor tin middling ore |
| CN102925673A (en) * | 2012-10-29 | 2013-02-13 | 云南锡业集团有限责任公司研究设计院 | Method for treating high-iron low-tin ores |
| CN104164572A (en) * | 2014-08-25 | 2014-11-26 | 北京矿冶研究总院 | Method for recovering valuable metals in tailings |
| CN107151741A (en) * | 2017-06-06 | 2017-09-12 | 江苏省冶金设计院有限公司 | A kind of system and method for handling lead and zinc smelting dreg |
| CN107201442A (en) * | 2017-06-06 | 2017-09-26 | 江苏省冶金设计院有限公司 | A kind of system and method for handling zinc leaching residue |
| CN107739817A (en) * | 2017-10-10 | 2018-02-27 | 北京矿冶研究总院 | Method for calcified chlorination and volatilization comprehensive resource utilization of jarosite slag |
| CN108486384A (en) * | 2018-03-16 | 2018-09-04 | 湖南腾驰环保科技有限公司 | The recovery process of low-grade stanniferous bismuth tungsten slag |
| CN109338111A (en) * | 2018-11-27 | 2019-02-15 | 贵州省兴安环保科技有限公司 | A method of from recycling valuable metal in material containing zinc-tin |
| CN112591831A (en) * | 2020-12-04 | 2021-04-02 | 兰州有色冶金设计研究院有限公司 | Harmless treatment method for strongly acidic mine tailings |
| CN112877537A (en) * | 2021-01-13 | 2021-06-01 | 何良东 | Method and system for high-temperature chlorination treatment of solid waste |
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Application publication date: 20100728 |