CN101979684A - Process for recovering zinc from hot-dip coating zinc ash - Google Patents
Process for recovering zinc from hot-dip coating zinc ash Download PDFInfo
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- CN101979684A CN101979684A CN2010105673993A CN201010567399A CN101979684A CN 101979684 A CN101979684 A CN 101979684A CN 2010105673993 A CN2010105673993 A CN 2010105673993A CN 201010567399 A CN201010567399 A CN 201010567399A CN 101979684 A CN101979684 A CN 101979684A
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Abstract
The invention relates to a process for recovering zinc from hot-dip coating zinc ash. The process comprises the following steps of: separating the hot-dip coating zinc ash after dry grinding and screening to obtain an oversize product and an undersize product; removing bound water and a small amount of zinc chloride from the oversize product under the condition that the temperature is between 400 and 500 DEG C and the vacuum degree is 10 to 50 Pa; performing vacuum distillation on the oversize product under the condition that the temperature is between 650 and 800 DEG C and the vacuum degree is 10 to 30 Pa to obtain zinc; and performing alkali cleaning on the undersize product to remove chlorine, and then performing vacuum thermal reduction on the undersize product to obtain the zinc from zinc oxide by using ferrosilicon as a reducing agent and calcium oxide as a slagging agent under the condition that the vacuum degree is 10 to 30 Pa and the temperature is between 1,050 and 1,200 DEG C. The process has a high recovery rate for recovering the zinc from the hot-dip coating zinc ash, and the obtained zinc has a good crystallized shape.
Description
Technical field
The present invention relates to the zinc secondary resource and reclaim the field, particularly a kind of technology that from the hot dip zinc gray, reclaims zinc.
Background technology
The whole world is used for the zinc amount that pot galvanize consumes every year and accounts for zinc total amount consumed 50%, has 20% metallic zinc to form zinc gray in hot galvanizing process approximately.Zinc gray zinc bath surface in the hot dip process contacts oxidized with atmosphere and floats over bath surface formation, and it mainly is made up of zinc oxide, metallic zinc and zinc chloride.The massfraction of zinc element is between 50%～85% in the general zinc gray.Zinc content height, the big zinc gray of total amount are if can not well be recycled the significant wastage that will cause zinc resource.Therefore along with the decline of primary zinc ore reserves and the continuous growth of zinc consumption, carry out the research of from zinc gray, reclaiming zinc, significant to the regeneration and the sustainable use thereof that realize zinc resource.
Existing hot dip zinc gray reclaims technology and mainly is divided into five kinds, is respectively:
1, roasting-acidleach-purification-electrolysis process.Zinc gray is separated the zinc oxide obtain 1200 ℃ of left and right sides high-temperature roastings through dry grinding, after muriate in the zinc gray (mainly being zinc chloride) steamed cl content in the zinc gray is removed to less than 0.05% (massfraction), the zinc oxide after the dechlorination through sulfuric acid leach, electrolysis obtains metallic zinc behind the electrolyte purification.This technology dechlorination cost is too high, and zinc loss amount is big in the dechlorination process, the loaded down with trivial details and electrolytic energy consumption height of the zinc (＞3000kwht of electrolyte purification technology
-1).
2, acidleach-removal of impurities-heavy zinc-acidleach-electrolysis process.Zinc gray with sulfuric acid dissolution after, in solution, add pure zinc oxide control pH value of solution value solution metal impurity precipitated under condition of different pH.Add yellow soda ash in the filtrate filtered, the zine ion in the solution is become the zinc carbonate precipitation.The zinc carbonate that obtains enters electrolysis process after with sulfuric acid dissolution and obtains metallic zinc.The yellow soda ash reagent that this processes expend is a large amount of, the production cost height, the production cycle is long, in industrial application difficult.The electrolytic energy consumption of zinc also＞3000kwht
-1
3, horizontal jar smelting process.Zinc gray with pack into after coke mixes in horizontal jar, jar is placed in the distilling furnace on the carriage, with 1250～1300 ℃ furnace gases tank body is carried out outer heating, behind CO gas that produces in jar and the zinc fume importing condenser, zinc vapor condensation becomes liquid Zn.Remaining zinc fume enters in the stretcher with CO, further reclaims zinc with " blue powder " form.The regenerated zinc quality that this technology obtains is low, generally can only reach No. 4 or No. 5 zinc, and zinc recovery is low only to be 40～60%.
4, airtight blast furnace smelting process.Zinc gray is after rotary kiln evaporation roasting dechlorination, allocating coke into is pressed into agglomerate and sends into melting in the blast furnace again, emit slag from the blast furnace bottom, the zinc fume that overflows from stove top is introduced the lead-splash condenser, isolates crude zinc after the zinc fume that is absorbed by plumbous rain is cooled in the cooling chute.This technology dechlorination cost height, and the material amount of carrying secretly causes greatly, and zinc vapor condensation efficient is low, zinc product purity is low.
5, preparation zinc chemical product.Zinc gray is directly prepared zinc chemical product as raw material, and as zinc chloride, zinc sulfate etc., not only cost is higher, and sales difficulty.
Generally speaking, existing processes all has place not fully up to expectations.At present, the hot dip zinc gray that presses for a kind of environment-friendly high-efficiency of exploitation reclaims technology.
Summary of the invention
The purpose of this invention is to provide that a kind of production energy consumption is lower, crystallization shape is good, reaction reduction ratio height, and does not almost have environmental pollution, hot dip zinc gray that labour intensity is little to reclaim technology, thereby overcome the defective of existing hot dip zinc gray recovery method.
Technical scheme of the present invention is: the hot dip zinc gray obtains containing metal zinc screen overflow and contains the zinc oxide screen underflow, thereby hot dip zinc gray metallic zinc and zinc oxide are carried out initial gross separation by dry grinding, the separation of screening back; Screen overflow is 400～500 ℃ in temperature, and vacuum tightness is to take off combination water and zinc chloride processing under 10～50Pa, is 650 ℃～800 ℃ in temperature then, and vacuum tightness is that vacuum distilling obtains metallic zinc under 10～30Pa condition; After the screen underflow process alkali cleaning dechlorination, utilize ferrosilicon to be reductive agent, calcium oxide is a slag former, is that 10～30Pa, temperature are under 1050～1200 ℃ of conditions in vacuum tightness, by vacuum-thermal reduction zinc oxide is got metallic zinc.
The screen overflow that obtains by dry grinding, screening is mainly metallic zinc, also contains zinc oxide and a spot of basic zinc chloride, and screen underflow is mainly zinc oxide, also contains basic zinc chloride.
Technical process is seen shown in the accompanying drawing 1.
Concrete steps of the present invention are as follows:
(1) the hot dip zinc gray is crossed the separation of 90-110 mesh sieve after dry grinding and obtain containing metal zinc screen overflow and contain the zinc oxide screen underflow, thereby hot dip zinc gray metallic zinc and zinc oxide are carried out initial gross separation;
(2) screen overflow is at 400～500 ℃, and vacuum tightness is 10～50Pa, and the time is after removing combination water and a small amount of zinc chloride of containing under 30～50min condition, to make agglomerate; The lumps raw material is put into vacuum oven, and to keep furnace pressure be 10～30Pa, be warming up to 650 ℃～800 ℃, distillation 30～50min; On condenser, obtain metallic zinc; Obtaining after the distillation sneaked into screen underflow and reclaimed to be mainly the residue of zinc oxide after dry grinding;
(3) screen underflow is made agglomerate after mixing with reductive agent ferrosilicon powder, slag former active calcium oxide and Calcium Fluoride (Fluorspan) after the alkali cleaning dechlorination; The lumps raw material is put into vacuum oven, and to keep furnace pressure be 10～30Pa, be warming up to 1050 ℃～1200 ℃, 60～150min; On condenser, obtain metallic zinc;
The a small amount of zinc chloride that removes 400～500 ℃ of vacuum distillings in described (2) step can be used to prepare the zinc chloride product and sell.
Reacted slag main component is 2CaOSiO in described (3) step
2, be one of main component of cement, can be used as the raw material of preparation cement.
The present invention compared with prior art has the following advantages:
(1) technology provided by the invention separately reclaims metallic zinc in the zinc gray and zinc oxide.Metallic zinc utilizes vacuum distilling to reclaim, and rate of recovery height, energy consumption is low, zinc product purity is higher.Zinc oxide adopts alkali cleaning-vacuum silicothermic process to reclaim zinc, and the alkali cleaning dechlorination has that equipment is simple, flow process short, low power consumption and other advantages.Utilize ferrosilicon as reductive agent, the material amount of carrying secretly is little in the reaction process, zinc vapor condensation efficient height, and the reduction ratio height of zinc, the product crystallization shape is good.
(2) effective utilization that all end products can both obtain among the present invention, Atom economy is good.
(3) production process of the present invention is finished in enclosed vacuum equipment, can not pollute, and production environment close friend, labour intensity is little.
(4) the present invention is the industrial renovation process of a kind of efficient, cleaning, environmental protection, also can be used to handle as chloride zinc secondary resources such as zinc casting type scum silica frost.
Description of drawings
Accompanying drawing 1 is the schema of technology of the present invention.
Embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
Zinc gray is crossed 100 mesh sieves after dry grinding, screening obtains screen overflow and screen underflow.Take by weighing the 10.00g screen overflow, the vacuum oven of packing into is 35Pa in vacuum tightness, after temperature is 450 ℃ of following constant temperature 30min, takes out and steams excess matter in the vacuum oven, makes agglomerate.Block raw material is put into vacuum oven, and vacuum tightness is 10Pa in the stove, and temperature is to distill 30min under 750 ℃ of conditions, recyclablely obtains the metallic zinc that quality is 5.60g, and the quality of residue is 3.30g.Residue is a zinc oxide through its main component of XRD analysis.Get the 10.00g screen underflow and obtain filter residue through the alkali cleaning after-filtration.Main component is a zinc oxide in the filter residue, take by weighing the 4.05g filter residue, filter residue and 2.80g calcium oxide, 1.16g75 ferrosilicon powder and 0.25g Calcium Fluoride (Fluorspan), make agglomerate through after mixing, block raw material is put into vacuum oven, vacuum tightness is 20Pa, is warming up to 1175 ℃ in the stove, 120min, and the quality that obtains reguline metal zinc is 2.55g.Reaction back residue quality is 4.75g, and main component is 2CaOSi0
2, wherein the zinc element massfraction is 4.25%.Reduction ratio by calculating silicothermic process when reduction zinc is 92.81%.
Embodiment 2
Zinc gray is crossed 100 mesh sieves after dry grinding, screening obtains screen overflow and screen underflow.Take by weighing the 10.00g screen overflow, the vacuum oven of packing into is 35Pa in vacuum tightness, and temperature is after distilling 30min under 450 ℃, to take out and steam excess matter in the vacuum oven, makes agglomerate.Block raw material is put into vacuum oven, and vacuum tightness is 10Pa, is warming up to 800 ℃ in the stove, and distillation 50min obtains the metal that quality is 5.75g (purity is 99.84%), and the quality of residue is 3.26g.Residue is a zinc oxide through its main component of XRD analysis.Get the 10.00g screen underflow and obtain filter residue through the alkali cleaning after-filtration.Main component is a zinc oxide in the filter residue, takes by weighing 4.05g filter residue and 2.80g calcium oxide, No. 75 ferrosilicon powders of 1.16g and 0.25g Calcium Fluoride (Fluorspan), makes agglomerate after mixing.Block raw material is put into vacuum oven, and vacuum tightness is 20Pa, is warming up to 1150 ℃ in the stove, reduction 60min, and obtaining quality is the reguline metal zinc of 2.21g, and reaction back residue quality is 5.20g, and wherein entrapped zinc element massfraction is 11.58%.Reduction ratio by calculating silicothermic process when reduction zinc is 78.79%.
Embodiment 3
Zinc gray is crossed 100 mesh sieves after dry grinding, screening obtains screen overflow and screen underflow.Take by weighing the 10.00g screen overflow, the vacuum oven of packing into is 35Pa in vacuum tightness, after temperature is 450 ℃ of following constant temperature 30min, takes out and steams excess matter in the vacuum oven, makes agglomerate.Block raw material is put into vacuum oven, and vacuum tightness is 10Pa, is warming up to 800 ℃ in the stove, distillation 40min, and the recyclable metal that quality is 5.71g (purity is 99.84%) that obtains, the quality of residue is 3.21g.Residue is a zinc oxide through its main component of XRD analysis.Get the 10.00g screen underflow and obtain filter residue through the alkali cleaning after-filtration.Main component is a zinc oxide in the filter residue, take by weighing 4.05g filter residue and 2.80g calcium oxide, 1.16g75 ferrosilicon powder and 0.25g Calcium Fluoride (Fluorspan), after mixing, make agglomerate, block raw material is put into vacuum oven, vacuum tightness is that 20Pa is warming up to 1100 ℃ in the stove, reduction 120min obtains the reguline metal zinc that quality is 1.45g, and reaction back residue quality is 6.08g, and wherein entrapped zinc element massfraction is 21.54%.Reduction ratio by calculating silicothermic process when reduction zinc is 53.84%.
Embodiment 4
Zinc gray is crossed 100 mesh sieves after dry grinding, screening obtains screen overflow and screen underflow.Take by weighing the 10.00g screen overflow, the vacuum oven of packing into is 35Pa in vacuum tightness, and temperature is after distilling 30min under 450 ℃, to take out and steam excess matter in the vacuum oven, makes agglomerate.Block raw material is put into vacuum oven, and vacuum tightness is 10Pa, is warming up to 700 ℃ in the stove, and distillation 40min obtains the metal that quality is 5.25g (purity is 99.84%), and the quality of residue is 3.68g.Residue is a zinc oxide through its main component of XRD analysis.Get the 10.00g screen underflow and obtain filter residue through the alkali cleaning after-filtration.Main component is a zinc oxide in the filter residue, takes by weighing 4.05g filter residue and 2.80g calcium oxide, No. 75 ferrosilicon powders of 1.16g and 0.25g Calcium Fluoride (Fluorspan), makes agglomerate after mixing.Block raw material is put into vacuum oven, and vacuum tightness is 20Pa, is warming up to 1075 ℃ in the stove, reduction 120min, and obtaining quality is the reguline metal zinc of 1.06g, and reaction back residue quality is 6.38g, and wherein entrapped zinc element massfraction is 27.53%.Reduction ratio by calculating silicothermic process when reduction zinc is 38.1%.
Claims (6)
1. a technology that reclaims zinc from the hot dip zinc gray is characterized in that, the hot dip zinc gray obtains containing metal zinc screen overflow and contains the zinc oxide screen underflow, thereby hot dip zinc gray metallic zinc and zinc oxide are carried out initial gross separation by dry grinding, the separation of screening back; Screen overflow is 400～500 ℃ in temperature, and vacuum tightness is to take off combination water and zinc chloride processing under 10～50Pa, is 650 ℃～800 ℃ in temperature then, and vacuum tightness is that vacuum distilling obtains metallic zinc under 10～30Pa condition; After the screen underflow process alkali cleaning dechlorination, utilize ferrosilicon to be reductive agent, calcium oxide is a slag former, is that 10～30Pa, temperature are under 1050～1200 ℃ of conditions in vacuum tightness, by vacuum-thermal reduction zinc oxide is got metallic zinc.
2. a kind of technology that reclaims zinc from the hot dip zinc gray according to claim 1 is characterized in that, the hot dip zinc gray is crossed 90-110 mesh sieve branch after dry grinding.
3. a kind of technology that reclaims zinc from the hot dip zinc gray according to claim 1 and 2 is characterized in that, may further comprise the steps:
(1) the hot dip zinc gray is crossed 90-110 mesh sieve branch after dry grinding, separate obtaining containing metal zinc screen overflow and containing the zinc oxide screen underflow, thereby hot dip zinc gray metallic zinc and zinc oxide are carried out initial gross separation;
(2) screen overflow is at 400～500 ℃, and vacuum tightness is 10～50Pa, and the time is after removing combination water and a small amount of zinc chloride of containing under 30～50min condition, to make agglomerate; The lumps raw material is put into vacuum oven, and to keep furnace pressure be 10～30Pa, be warming up to 650 ℃～800 ℃, distillation 30～50min; On condenser, obtain metallic zinc;
(3) screen underflow is made agglomerate after mixing with reductive agent ferrosilicon powder, slag former active calcium oxide and Calcium Fluoride (Fluorspan) after the alkali cleaning dechlorination; The lumps raw material is put into vacuum oven, and to keep furnace pressure be 10～30Pa, be warming up to 1050 ℃～1200 ℃, 60～150min; On condenser, obtain metallic zinc.
4. a kind of technology that reclaims zinc from the hot dip zinc gray according to claim 3 is characterized in that obtaining after the distillation is mainly the residue of zinc oxide, sneaks into screen underflow and reclaim after dry grinding.
5. according to claim 3 or 4 described a kind of technologies that from the hot dip zinc gray, reclaim zinc, it is characterized in that the zinc chloride that removes 400～500 ℃ of vacuum distillings in described (2) step is used to prepare the zinc chloride product.
6. according to claim 3 or 4 described a kind of technologies that from the hot dip zinc gray, reclaim zinc, it is characterized in that reacted slag is as the raw material of preparation cement in described (3) step.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468960A (en) * | 2013-08-23 | 2013-12-25 | 佛山市诺傲再生资源科技有限公司 | Process equipment for dedusted zinc ash and process method thereof |
| CN103602828A (en) * | 2013-10-15 | 2014-02-26 | 武汉钢铁(集团)公司 | Method and device for producing zinc alloy used for hot dipping by using zinc slag |
| CN103993182A (en) * | 2014-05-07 | 2014-08-20 | 西安建筑科技大学 | Comprehensive recovery method for secondary resources in iron vitriol slag |
| CN106811602A (en) * | 2017-02-20 | 2017-06-09 | 石家庄学院 | A kind of method that utilization cadmia prepares zinc oxide |
| CN107385230A (en) * | 2017-07-31 | 2017-11-24 | 重庆科技学院 | A kind of steel-making dust recoverying and utilizing method and its vacuum reduction furnace equipment used |
| CN107557590A (en) * | 2017-09-07 | 2018-01-09 | 湖南三立集团股份有限公司 | Zinc dross recoverying and utilizing method |
| CN107760882A (en) * | 2017-09-30 | 2018-03-06 | 重庆科技学院 | The method that zinc in Electric Cooker comminuted steel shot dirt is refined using industrial dust containing calcium oxide |
| CN108179283A (en) * | 2018-01-23 | 2018-06-19 | 昆明理工大学 | A kind of continuous vacuum distillation equipment and its application process for handling hot galvanizing residue or zinc-tin powder |
| CN108220640A (en) * | 2016-12-13 | 2018-06-29 | 鞍钢股份有限公司 | A kind of method that hot dip kirsite is manufactured with cadmia |
| CN110172590A (en) * | 2019-05-31 | 2019-08-27 | 唐山鑫联环保科技有限公司 | A method of promote chlorine in high chlorine Zinc Oxide to remove using solid phase reaction |
| CN111733333A (en) * | 2020-01-15 | 2020-10-02 | 马鞍山马钢废钢有限责任公司 | Dezincification method for galvanized steel scrap |
| CN113444887A (en) * | 2021-06-29 | 2021-09-28 | 海西华汇化工机械有限公司 | Resource utilization method for preparing zinc-nickel alloy by using zinc ash |
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| CN1323909A (en) * | 2000-05-11 | 2001-11-28 | 中南工业大学 | Method of extracting zinc from zine slag |
| CN1421535A (en) * | 2001-11-23 | 2003-06-04 | 宝山钢铁股份有限公司 | Regeneration process of zinc residue produced in hot zinc plating |
| WO2006133777A1 (en) * | 2005-06-13 | 2006-12-21 | Umicore | Separation of metal values in zinc leaching residues |
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- 2010-12-01 CN CN2010105673993A patent/CN101979684B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1323909A (en) * | 2000-05-11 | 2001-11-28 | 中南工业大学 | Method of extracting zinc from zine slag |
| CN1421535A (en) * | 2001-11-23 | 2003-06-04 | 宝山钢铁股份有限公司 | Regeneration process of zinc residue produced in hot zinc plating |
| WO2006133777A1 (en) * | 2005-06-13 | 2006-12-21 | Umicore | Separation of metal values in zinc leaching residues |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468960B (en) * | 2013-08-23 | 2015-05-06 | 佛山市诺傲再生资源科技有限公司 | Process equipment for dedusted zinc ash and process method thereof |
| CN103468960A (en) * | 2013-08-23 | 2013-12-25 | 佛山市诺傲再生资源科技有限公司 | Process equipment for dedusted zinc ash and process method thereof |
| CN103602828A (en) * | 2013-10-15 | 2014-02-26 | 武汉钢铁(集团)公司 | Method and device for producing zinc alloy used for hot dipping by using zinc slag |
| CN103993182A (en) * | 2014-05-07 | 2014-08-20 | 西安建筑科技大学 | Comprehensive recovery method for secondary resources in iron vitriol slag |
| CN108220640A (en) * | 2016-12-13 | 2018-06-29 | 鞍钢股份有限公司 | A kind of method that hot dip kirsite is manufactured with cadmia |
| CN108220640B (en) * | 2016-12-13 | 2019-12-13 | 鞍钢股份有限公司 | Method for manufacturing zinc alloy for hot dipping by using zinc slag |
| CN106811602A (en) * | 2017-02-20 | 2017-06-09 | 石家庄学院 | A kind of method that utilization cadmia prepares zinc oxide |
| CN107385230A (en) * | 2017-07-31 | 2017-11-24 | 重庆科技学院 | A kind of steel-making dust recoverying and utilizing method and its vacuum reduction furnace equipment used |
| CN107557590A (en) * | 2017-09-07 | 2018-01-09 | 湖南三立集团股份有限公司 | Zinc dross recoverying and utilizing method |
| CN107760882A (en) * | 2017-09-30 | 2018-03-06 | 重庆科技学院 | The method that zinc in Electric Cooker comminuted steel shot dirt is refined using industrial dust containing calcium oxide |
| CN107760882B (en) * | 2017-09-30 | 2018-09-21 | 重庆科技学院 | The method for refining zinc in Electric Cooker comminuted steel shot dirt using industrial dust containing calcium oxide |
| CN108179283A (en) * | 2018-01-23 | 2018-06-19 | 昆明理工大学 | A kind of continuous vacuum distillation equipment and its application process for handling hot galvanizing residue or zinc-tin powder |
| CN110172590A (en) * | 2019-05-31 | 2019-08-27 | 唐山鑫联环保科技有限公司 | A method of promote chlorine in high chlorine Zinc Oxide to remove using solid phase reaction |
| CN110172590B (en) * | 2019-05-31 | 2021-07-20 | 唐山鑫联环保科技有限公司 | Method for promoting chlorine removal in high-chlorine zinc oxide powder by adopting solid-phase reaction |
| CN111733333A (en) * | 2020-01-15 | 2020-10-02 | 马鞍山马钢废钢有限责任公司 | Dezincification method for galvanized steel scrap |
| CN113444887A (en) * | 2021-06-29 | 2021-09-28 | 海西华汇化工机械有限公司 | Resource utilization method for preparing zinc-nickel alloy by using zinc ash |
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