CN103320623B - The method of a kind of steam activation/microwave calcining zinc oxide fumes dechlorination and device - Google Patents
The method of a kind of steam activation/microwave calcining zinc oxide fumes dechlorination and device Download PDFInfo
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- CN103320623B CN103320623B CN201310283666.8A CN201310283666A CN103320623B CN 103320623 B CN103320623 B CN 103320623B CN 201310283666 A CN201310283666 A CN 201310283666A CN 103320623 B CN103320623 B CN 103320623B
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Abstract
The present invention relates to method and the device of a kind of steam activation/microwave calcining zinc oxide fumes dechlorination, belong to technical field of wet metallurgy.The method carries out roasting under zinc oxide fumes powder being placed in sealed microwave condition, blast air in atmospheric conditions and pass into water vapour, and the gas produced is discharged, the temperature of Zn dust powder to be oxidized is elevated to 500 ~ 750 DEG C, insulation 20 ~ 180min, the zinc oxide fumes powder after dechlorinating is obtained, dechlorination rate > 93wt% after naturally cooling.Device comprises airtight microwave reaction device and air-breathing and refining plant, the structure of air-breathing and refining plant is communicated with dust suction bottle, scrubbing bottle, surge flask and micro-suction pump successively by conduit, microwave reaction device is communicated with dust suction bottle by conduit, and chlorine economical and effective in zinc oxide fumes can be removed with water vapour and gas inlet, zinc oxide fumes after treatment directly can leach in wet processing, reduce chlorine impurity to the impact of electric zinc production process, improve the recovery utilization rate of secondary resource.
Description
Technical field
The present invention relates to method and the device of a kind of steam activation/microwave calcining zinc oxide fumes dechlorination, belong to technical field of wet metallurgy.
Background technology
Zinc oxide fumes is important zinc secondary resource, mainly contain the zinc oxide fumes of zinc hydrometallurgy leached mud through rotary kiln reduction volatilization output, the zinc oxide fumes that plumbum smelting slag obtains through fuming furnace smelting technology, the byproduct zinc oxide fumes that brass metallurgical slag and copper material source mill smelting system reclaim, zinc-plated iron-steel gives up the zinc oxide fumes that electric arc furnace flue dust that part produces in removal process obtains through rotary kiln reducing roasting, blast furnace dust or gas mud are multiple through the Second-rate zinc oxide powder etc. of Webster stove process output, these zinc oxide fumeses are containing zinc 40 ~ 60%, leaded 10 ~ 20%, also containing a small amount of cadmium, zinc oxide fumes per ton contains the indium of 600 ~ 1000g, there is certain Development volue and profit margin, therefore many zinc abstraction enterprises take zinc oxide fumes as the recycling of raw material production electricity zinc and valuable metal, but in process of production, these enterprises without exception encounter identical problem: the fault caused that exceeds standard of the chlorion in electric effusion is difficult to overcome.In electrolytic deposition process, the existence of chlorine impurity will cause the corrosion of positive plate, too increase plumbum ion concentration in electrolytic solution simultaneously, the rapid rising of zinc cathode consumption, in addition, chlorion is circulation collection in wet smelting process, increasing of chlorine makes sulfate system void tower, packing tower, it is more serious that drying tower goes out acid tube corrosion, cause spray acid distributed pole uneven, impact purification, drying and assimilation effect, corrode the equipment such as blower fan simultaneously, also to some extent corrosion is created to the porcelain filling in each tower, cause catalyst efflorescence, larger difficulty is brought to production, electrolysis cost is raised, impact is normal produces, Eletrolytic zinc quality is caused to decline, even stopping production accident can be caused time serious.
At present, be in the technique of raw material production electricity zinc with zinc oxide fumes, the technological line removing chlorine has two: one to be adopt pretreated mode, namely before leaching, carries out pre-treatment to raw material and removes chlorine.Its dechlorination technology has that roasting removes chlorine, neutralizing treatment removes and the vitriol oil removes the methods such as chlorine.The method that industrial roasting removes chlorine mainly multiple hearth furnace roasting removes, but multiple hearth furnace equipment is huge, and one-time investment is high, energy consumption is high, and equipment is fragile and maintenance cost is high, for the zinc oxide fumes that the detrimental impurity such as chlorine are higher, chlorine pressure in multiple hearth furnace also can be caused suddenly to increase, and removal effect is not good enough.And its drawback of the method for neutralizing treatment and vitriol oil dechlorination to be material smoke components after process have to pass through suitable process and just can reach emission standard, and intractability is large and bring higher processing cost.Two is directly leached by zinc oxide fumes, makes fluorine chlorine enter solution, then de-fluorine and chlorine removal from solution of zinc sulfate.Main methods has ion-exchange dechlorination method, extraction dechlorination method, pyrrhosiderite dechlorination method, zinc sulfate crystalline deposit method, cuprous chloride dechlorination method etc.See with regard to its art breading feature, such treatment process is all due to deficiencies such as processing cost are high, energy consumption is high, treatment scheme is long.The ubiquitous deficiency of these removing sulfuldioxide brings the problem of restriction to the process of subsequent technique.
Therefore, how cost-effective chlorine in zinc oxide fumes to be removed, solve electric zinc and to produce and restriction problem in valuable metal recovery process is the difficult problem needing to be explored.
Summary of the invention
The present invention is directed to the deficiency of existing chlorine removing process, method and the device of a kind of steam activation/microwave calcining zinc oxide fumes dechlorination are provided, chlorine economical and effective in zinc oxide fumes can be removed, zinc oxide fumes after treatment directly can leach in wet processing, reduce chlorine impurity to the impact of electric zinc production process, improve the recovery utilization rate of secondary resource.
Technical scheme of the present invention is: carry out roasting under zinc oxide fumes powder being placed in sealed microwave condition, blast air in atmospheric conditions and pass into water vapour, the process of roasting stirs zinc oxide fumes powder, and the gas produced is discharged, the temperature of Zn dust powder to be oxidized is elevated to 500 ~ 750 DEG C, insulation 20 ~ 180min, obtains the zinc oxide fumes powder after dechlorinating, dechlorination rate > 93wt% after naturally cooling.
Described zinc oxide fumes powder is a kind of flue dust of breeze leached mud through rotary kiln evaporation output, zinc oxide fumes powder is containing zinc oxide 60 ~ 80wt%, plumbous 10 ~ 15wt%, iron 1 ~ 5wt%, rare loose half a lifetime indium metal 0.05 ~ 0.2wt%, detrimental impurity chlorine 0.1 ~ 0.9wt%, all the other are impurity; Smoke granularity is 0.5 ~ 4 μm.
The frequency of described microwave calcining is 2400 ~ 2500MHz, output rating is 0.1 ~ 2kW/kg.
The vapor flow that the air flow quantity that described per kilogram zinc oxide fumes powder blasts is 500 ~ 1500L/h, pass into is 1 ~ 150mL/min.
Described zinc oxide fumes powder remains on 1 ~ 100 DEG C/min through the temperature rise rate of heated under microwave conditions.
The speed that described zinc oxide fumes powder stirs in the process of microwave calcining is 5 ~ 120r/min.
The gas that described zinc oxide fumes powder produces in the process of microwave calcining is HCl, reclaims successively after discharge through washing and alkali cleaning.The solution of alkali cleaning is sodium carbonate solution or sodium hydroxide solution.
The structure of apparatus of the present invention is: comprise airtight microwave reaction device and air-breathing and refining plant, the structure of air-breathing and refining plant is communicated with dust suction bottle 9, scrubbing bottle 10, surge flask 11 and micro-suction pump 12 successively by conduit, microwave reaction device is communicated with dust suction bottle 9 by conduit, and with water vapour and gas inlet 1; The conduit access of dust suction bottle 9, scrubbing bottle 10 and surge flask 11 be all according to progress short go out mode distribute.
The body of described microwave reaction device is the airtight microwave cavity 8 with micro-wave energy generating unit 5, and microwave cavity 8 inside has and is provided with agitator 3 and measuring and controlling temp device 2 with in the vessel of heat-insulation material 7, vessel.
Described scrubbing bottle 10 has 2 at least, and the gas that reaction produces needs successively through washing and alkali cleaning.
The using method of apparatus of the present invention: accurately take zinc oxide fumes raw material, load the vessel with heat-insulation material 7, all be placed in airtight microwave cavity 8, and the appropriate location that agitator 3 and the thermopair of measuring and controlling temp device 2 are placed in vessel is fully contacted with material, adopt tubes connection microwave cavity 8 and air-breathing and refining plant, after inspection units connects, open micro-wave energy generating unit 5 successively, stirring system 3 and tail gas absorbing system micro-suction pump 12, regulate microwave generating apparatus 5, control microwave frequency is 2400 ~ 2500MHz, output rating is 0.1 ~ 2kW/kg.Roasting process passes into air in reaction vessels, the mode that water vapour is carried by air enters microwave reaction vessel from water vapour and gas inlet 1 through conduit, the process of steam activation microwave calcining is carried out to material, by regulate microwave generating apparatus 5, vapor flow, stirring velocity, research specified temp and soaking time under roasting dechlorination effect.
The invention has the beneficial effects as follows: the principle utilizing the metal chloride of contained valuable metal in zinc oxide fumes and a small amount of sulphur content and water vapour to react, makes ZnCl
2, PbCl
2solid slag is formed with the form of oxide compound and vitriol Deng the metal ion in metal chloride, chlorine then volatilizees with the form of HCl gas, in roasting process, continuously stirring is carried out to material, continuous air extraction operation is carried out to microwave cavity simultaneously, the HCl gas generated can be discharged washing absorption timely, zinc oxide fumes after treatment directly can leach recycling in wet processing, reduce chlorine impurity to the impact of electric zinc production process, good condition is created in the recovery for valuable metal; After steam-activation treatment zinc oxide fumes microwave calcining, chlorine extrusion rate is high, dechlorination rate > 93%; The microwave calcining equipment mature and reliable that the present invention relates to, simple to operation, level of automation is high, and electrolysis utilization ratio is high, the advantages such as economic environmental protection.
Accompanying drawing explanation
Fig. 1 is device schematic diagram of the present invention.
In figure, each label is: 1-water vapour and gas inlet, 2-measuring and controlling temp device, 3-agitator, 4-control damper, 5-micro-wave energy generating unit, 6-zinc oxide fumes powder, 7-heat-insulation material, 8-microwave cavity, 9-dust suction bottle, 10 scrubbing bottles, 11-surge flask, 12-micro-suction pump.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment one: the method for the steam activation/microwave calcining zinc oxide fumes dechlorination of the present embodiment is: (composition of zinc oxide fumes powder is zinc oxide 60wt%, plumbous 15wt%, iron 5wt% by zinc oxide fumes powder, indium trioxide 0.1wt%, chlorine 0.9wt%, all the other are impurity, granularity is 2 ~ 4 μm) be placed in sealed microwave condition under carry out roasting (frequency be 2400MHz, output rating is 2kW/kg), blast air in atmospheric conditions and pass into water vapour (air flow quantity that per kilogram zinc oxide fumes powder blasts is 500L/h, the vapor flow passed into is 27mL/min), the process of roasting is stir under the condition of 120r/min in speed to zinc oxide fumes powder, and the gas produced is discharged, temperature rise rate remains on 65 DEG C/min, the temperature of Zn dust powder to be oxidized is elevated to 650 DEG C, insulation 180min, the zinc oxide fumes powder after dechlorination is obtained after naturally cooling.
The device of the steam activation/microwave calcining zinc oxide fumes dechlorination of the present embodiment comprises airtight microwave reaction device and air-breathing and refining plant, the structure of air-breathing and refining plant is communicated with dust suction bottle 9, scrubbing bottle 10, surge flask 11 and micro-suction pump 12 successively by conduit, microwave reaction device is communicated with dust suction bottle 9 by conduit, and with water vapour and gas inlet 1; The conduit access of dust suction bottle 9, scrubbing bottle 10 and surge flask 11 be all according to progress short go out mode distribute.The body of microwave reaction device is the airtight microwave cavity 8 with micro-wave energy generating unit 5, and microwave cavity 8 inside has and is provided with agitator 3 and measuring and controlling temp device 2 with in the vessel of heat-insulation material 7, vessel.Scrubbing bottle 10 has 2, is followed successively by alkali cleaning bottle and pickling bottle.
The decreasing ratio of the zinc oxide fumes chlorine after adopting the device as Fig. 1 to carry out steam activation-microwave calcining process reaches 93.28%, its cl content reaches flowsheet of wet zinc smelting zinc oxide fumes and leaches requirement, can directly return wet-leaching flow process by the zinc oxide fumes after present method process.
Embodiment two: the method for the steam activation/microwave calcining zinc oxide fumes dechlorination of the present embodiment is: (composition of zinc oxide fumes powder is zinc oxide 80wt%, plumbous 13wt%, iron 1wt% by zinc oxide fumes powder, rare loose half a lifetime indium metal 0.05wt%, chlorine 0.1wt%, all the other are impurity, granularity is 0.5 ~ 3 μm) be placed in sealed microwave condition under carry out roasting (frequency be 2500MHz, output rating is 1kW/kg), blast air in atmospheric conditions and pass into water vapour (air flow quantity that per kilogram zinc oxide fumes powder blasts is 500L/h, the vapor flow passed into is 1mL/min), the process of roasting is stir under the condition of 100r/min in speed to zinc oxide fumes powder, and the gas produced is discharged, temperature rise rate remains on 100 DEG C/min, the temperature of Zn dust powder to be oxidized is elevated to 500 DEG C, insulation 20min, the zinc oxide fumes powder after dechlorination is obtained after naturally cooling, the decreasing ratio of chlorine is 93.41wt%, its cl content is far smaller than flowsheet of wet zinc smelting zinc oxide fumes and leaches requirement, wet-leaching flow process can be directly returned by the zinc oxide fumes after present method process.
The device of the steam activation/microwave calcining zinc oxide fumes dechlorination of the present embodiment comprises airtight microwave reaction device and air-breathing and refining plant, the structure of air-breathing and refining plant is communicated with dust suction bottle 9, scrubbing bottle 10, surge flask 11 and micro-suction pump 12 successively by conduit, microwave reaction device is communicated with dust suction bottle 9 by conduit, and with water vapour and gas inlet 1; The conduit access of dust suction bottle 9, scrubbing bottle 10 and surge flask 11 be all according to progress short go out mode distribute.Scrubbing bottle 10 has 4, is followed successively by two alkali cleaning bottles and two pickling bottles.
Embodiment three: the method for the steam activation/microwave calcining zinc oxide fumes dechlorination of the present embodiment is: (composition of zinc oxide fumes powder is zinc oxide 70wt%, plumbous 10wt%, iron 3wt% by zinc oxide fumes powder, rare loose half a lifetime indium metal 0.2wt%, chlorine 0.8wt%, all the other are impurity, granularity is 0.5 ~ 4 μm) be placed in sealed microwave condition under carry out roasting (frequency be 2450MHz, output rating is 0.1kW/kg), blast air in atmospheric conditions and pass into water vapour (air flow quantity that per kilogram zinc oxide fumes powder blasts is 1500L/h, the vapor flow passed into is 150mL/min), the process of roasting is stir under the condition of 5r/min in speed to zinc oxide fumes powder, and the gas produced is discharged, temperature rise rate remains on 1 DEG C/min, the temperature of Zn dust powder to be oxidized is elevated to 750 DEG C, insulation 120min, the zinc oxide fumes powder after dechlorination is obtained after naturally cooling, decreasing ratio 95.72wt%, its cl content is far smaller than flowsheet of wet zinc smelting zinc oxide fumes and leaches requirement, wet-leaching flow process can be directly returned by the zinc oxide fumes after present method process.
The device of the steam activation/microwave calcining zinc oxide fumes dechlorination of the present embodiment comprises airtight microwave reaction device and air-breathing and refining plant, the structure of air-breathing and refining plant is communicated with dust suction bottle 9, scrubbing bottle 10, surge flask 11 and micro-suction pump 12 successively by conduit, microwave reaction device is communicated with dust suction bottle 9 by conduit, and with water vapour and gas inlet 1; The conduit access of dust suction bottle 9, scrubbing bottle 10 and surge flask 11 be all according to progress short go out mode distribute.The body of microwave reaction device is the airtight microwave cavity 8 with micro-wave energy generating unit 5, and microwave cavity 8 inside has and is provided with agitator 3 and measuring and controlling temp device 2 with in the vessel of heat-insulation material 7, vessel.Scrubbing bottle 10 has 3, is followed successively by two alkali cleaning bottles and a pickling bottle.
Embodiment four: the zinc oxide fumes of chloride for 300g 0.236% being placed in microwave frequency is 2450MHz, it is roasting under the microwave condition of 3kW/kg that microwave exports specific power, roasting process passes into air in reaction vessel, control air flow quantity is 1000L/ (hkg), passes into water vapour with the flow velocity of 27mL/ (minkg) in reaction vessel simultaneously; Controlling temperature rise rate is 65 DEG C/min, after temperature arrives 650 DEG C, and insulation 60min; Muriate and activator water vapour are fully reacted and generates HCl gas; In roasting process, continuously stirring is carried out to material, and microwave cavity is bled, keep normal pressure, the HCl gas that timely eliminating roasting process produces, reach the object of zinc oxide fumes dechlorination, decreasing ratio reaches 93.11wt%, and its cl content reaches flowsheet of wet zinc smelting zinc oxide fumes and leaches requirement, can directly return wet-leaching flow process by the zinc oxide fumes after present method process.
Embodiment five: the zinc oxide fumes of chloride for 150kg 0.236% being placed in microwave frequency is 2450MHz, it is roasting under the microwave condition of 0.12kW/kg that microwave exports specific power, roasting process passes into air in reaction vessel, passes into water vapour with the flow velocity of 1.2mL/ (minkg) in reaction vessel; After temperature arrives 600 DEG C, insulation 120min; Muriate and activator water vapour are fully reacted and generates HCl gas; In roasting process, continuously stirring is carried out to material, and microwave cavity is bled, keep normal pressure, the HCl gas that timely eliminating roasting process produces, reach the object of zinc oxide fumes dechlorination, the decreasing ratio of chlorine reaches 93.41%, and its cl content is far smaller than flowsheet of wet zinc smelting zinc oxide fumes and leaches requirement, can directly return wet-leaching flow process by the zinc oxide fumes after present method process.
Embodiment six: the zinc oxide fumes of chloride for 180kg 0.236% being placed in microwave frequency is 2450MHz, it is roasting under the microwave condition of 0.1kW/kg that microwave exports specific power, roasting process passes into air in reaction vessel, passes into water vapour with the flow velocity of 1.2mL/ (minkg) in reaction vessel; After temperature arrives 700 DEG C, insulation 120min; Muriate and activator water vapour are fully reacted and generates HCl gas; In roasting process, continuously stirring is carried out to material, and microwave cavity is bled, keep normal pressure, get rid of the HCl gas that roasting process produces in time, reach the object of zinc oxide fumes dechlorination, the decreasing ratio 95.72wt% of chlorine.
Comparative example: the method for this comparative example microwave calcining zinc oxide fumes dechlorination is: the zinc oxide fumes of chloride for 300g 0.236% being placed in microwave frequency is 2450MHz, it is roasting under the microwave condition of 3kW/kg that microwave exports specific power, roasting process passes into air in reaction vessel, and control air flow quantity is 1300L/ (hkg); Controlling temperature rise rate is 65 DEG C/min, and after temperature arrives 650 DEG C, insulation 60min, finally obtains the zinc oxide fumes powder after dechlorination; In roasting process, continuously stirring is carried out to material, and microwave cavity is bled, keep normal pressure.The decreasing ratio 63.3% of chlorine after microwave calcining process.
Below by reference to the accompanying drawings the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (2)
1. the device of steam activation/microwave calcining zinc oxide fumes dechlorination, it is characterized in that: comprise airtight microwave reaction device and air-breathing and refining plant, the structure of air-breathing and refining plant is communicated with dust suction bottle (9), scrubbing bottle (10), surge flask (11) and micro-suction pump (12) successively by conduit, microwave reaction device is communicated with dust suction bottle (9) by conduit, and with water vapour and gas inlet (1); The conduit access of dust suction bottle (9), scrubbing bottle (10) and surge flask (11) be all according to progress short go out mode distribute; Described scrubbing bottle (10) has 2 at least, and the gas that reaction produces needs successively through washing and alkali cleaning.
2. the device of steam activation according to claim 1/microwave calcining zinc oxide fumes dechlorination, it is characterized in that: the body of described microwave reaction device is the airtight microwave cavity (8) with micro-wave energy generating unit (5), microwave cavity (8) inside has and is provided with agitator (3) and measuring and controlling temp device (2) with in the vessel of heat-insulation material (7), vessel.
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| CN104846217B (en) * | 2015-04-21 | 2017-01-04 | 昆明理工大学 | A kind of multiple ligand is combined coordination ammonia process and leaches the method and device of blast furnace dust recovery zinc |
| CN106289928A (en) * | 2016-10-11 | 2017-01-04 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method and apparatus that solid sample is carried out dechlorination de-carbon |
| CN107601547A (en) * | 2017-08-28 | 2018-01-19 | 中南大学 | The control method of remaining chlorinity in metal oxide |
| CN109052484B (en) * | 2018-10-25 | 2024-02-23 | 唐山学院 | Iron oxide powder dechlorination device and control method thereof |
| CN110184471B (en) * | 2019-07-15 | 2020-11-10 | 安徽工业大学 | Method for comprehensively recovering multiple elements enriched gold and silver precious metals from steel ash |
| CN112892176A (en) * | 2021-01-15 | 2021-06-04 | 北京单原子催化科技有限公司 | Recovery processing method of zinc in zinc oxide desulfurization waste agent |
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