CN103395825A - Method for producing nanometer zinc oxide by using steelmaking electric-furnace flue dust - Google Patents
Method for producing nanometer zinc oxide by using steelmaking electric-furnace flue dust Download PDFInfo
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- CN103395825A CN103395825A CN2013103359609A CN201310335960A CN103395825A CN 103395825 A CN103395825 A CN 103395825A CN 2013103359609 A CN2013103359609 A CN 2013103359609A CN 201310335960 A CN201310335960 A CN 201310335960A CN 103395825 A CN103395825 A CN 103395825A
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Abstract
The invention discloses a method for producing nanometer zinc oxide by using steelmaking electric-furnace flue dust. In order to solve the difficult recovery problem on the steelmaking electric-furnace flue dust in conventional steel plants, the method for producing nanometer zinc oxide by using the steelmaking electric-furnace flue dust comprises the following steps: 1) placing the steelmaking electric-furnace flue dust in concentrated sulfuric acid for complete reaction, filtering; 2) adding a PbO2 powder into a leaching liquor and fully stirring to remove impurities of Fe and Mn; 3) after filtering, adding zinc powder into the filtrate to remove impurities of Pb, Cu and Cd; 4) after filtering, adding ammonia water or an ammonium bicarbonate solution to generate a zinc-ammonia complex; and 5) drying the zinc-ammonia complex to generate nanometer zinc oxide. The method has the advantages of simple technology, low equipment investment and high recovery rate of zinc oxide.
Description
Technical field
The present invention relates to a kind of method of utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide.
Background technology
The chemical constitution of Steel Plant's steel-smelting electric furnace flue dust depends primarily on steel-making raw scrap material used, and general raw scrap material used contains zinc 15%～25%.China only had and just established dust arrester installation more than 50 tons past, but the flue dust of collecting do not utilize yet, and not only jeopardized environment, to resource, was also very large waste.Along with China's hot dip increases considerably with zinc, thereby the flue dust of recovery steel melting furnace realizes that regenerated zinc production seems particularly important.
Nano zine oxide is a kind of novel high function fine inorganic product, with conventional oxidation zinc, compares, and nano zine oxide has the incomparable property of general zinc oxide product and new purposes at aspects such as magnetic, light, electricity, sensitivities.In rubber, coating, printing ink, pigment, catalyzer, makeup and medicine and other fields, show more wide application prospect.
CN102826588A discloses the method for utilizing the decarburization of smoke of steel factory ash ammonia process to produce high-purity nm zinc oxide, comprise the following steps: leaching smoke of steel factory ash, purification and impurity removal, ammonia still process crystallization and drying and calcining is characterized in that: leaching smoke of steel factory ash leaches as leaching agent with ammoniacal liquor-ammonium fluid; Wherein, the volumetric molar concentration c (NH of NH3 in described leaching agent
3)=5.5-7mol/L, CO
3 2-Volumetric molar concentration c (CO
3 2-)=0.95-1.2mol/L, and in every cubic metre of leaching agent, add the 0.3-0.5kg Sodium Silicofluoride, after leaching, obtain leaching liquid; In the rear gained leaching liquid of leaching, zinc oxide concentration is controlled at 50-60g/L, the decarburization that heats up, and its method is: in every cubic metre of leaching liquid, add 50-60kg white lime, be heated with stirring to 90-98 ℃, work as CO
2Concentration≤0.3mol/L, add the 3-4kg ammonium persulphate in every cubic metre of aforementioned liquids, and add white lime 10kg/m
3Continue stir decarburization and oxidizing reaction occurs, until c (CO
2)≤0.1mol/L, then filtering separation; After purification and impurity removal, carry out refinement treatment, method is: in the liquid after purification and impurity removal is processed, add tensio-active agent, add-on is 30-50g tensio-active agent in the liquid after every cubic metre of purification and impurity removal is processed.
CN102826589A discloses the method for utilizing smoke of steel factory ash ammonia process to produce high-purity nm zinc oxide, comprise the following steps: leaching smoke of steel factory ash, purification and impurity removal, ammonia still process crystallization and drying and calcining, it is characterized in that: before leaching smoke of steel factory ash step, in pending smoke of steel factory ash, add white lime to obtain compound, and add water maintenance mixture moisture content 8-10%, then carry out admixture activation, the amount of the white lime that adds, by weight, be the 3-5% of smoke of steel factory ash; Smoke of steel factory after admixture activation ash is leached as leaching agent with ammoniacal liquor-ammonium fluid; Wherein, NH in described leaching agent
3Volumetric molar concentration c (NH3)=4.5-7mol/L, CO
3 2-Volumetric molar concentration c (CO
3 2-)=0.95-1.5mol/L, add the 0.3-0.5kg Sodium Silicofluoride in every cubic metre of leaching agent; After purification and impurity removal, carry out refinement treatment, method is: in the liquid after purification and impurity removal is processed, add ammonium phosphate and tensio-active agent, add-on is 1-3kg ammonium phosphate, 10-50g tensio-active agent in the liquid after every cubic metre of purification and impurity removal is processed.
CN102826586A discloses the method for utilizing the smoke of steel factory ash to produce high-purity nm zinc oxide, it is characterized in that, comprise the following steps: leaching smoke of steel factory ash, purification and impurity removal, ammonia still process crystallization and drying and calcining, it is characterized in that: during leaching smoke of steel factory ash, with ammoniacal liquor-ammonium fluid, as leaching agent, leach; Wherein, NH in described leaching agent
3Volumetric molar concentration c (NH
3)=4.5-7mol/L, CO
3 2-Volumetric molar concentration c (CO
3 2-)=0.95-1.5mol/L, and in every cubic metre of leaching agent, add the 0.3-0.5kg Sodium Silicofluoride, after leaching, obtain leaching liquid; Before the purification and impurity removal step, carry out pre-ammonia still process, method is: the leaching liquid that will obtain after leaching is heated to 95-105 ℃ and analyses ammonia, until c (NH in leaching liquid
3)≤3mol/L, then, by in the leaching liquid of every cubic metre, adding the 2-4kg ammonium persulphate and stirring oxidation, carry out solid-liquid separation by the liquid after pre-ammonia still process, and solution enters the purification and impurity removal step; After purification and impurity removal, carry out refinement treatment, method is: in the liquid after purification and impurity removal is processed, add ammonium phosphate and tensio-active agent, add-on is 1-3kg ammonium phosphate, 30-50g tensio-active agent in the liquid after every cubic metre of purification and impurity removal is processed.
But the method for prior art seems very difficult for the processing of the steel-smelting electric furnace flue dust that contains the impurity such as Mn, Cu, Cd, Ni.
Summary of the invention
In order to overcome the deficiency of existing Steel Plant steel-smelting electric furnace fume recovery difficulty, the present invention aims to provide a kind of method of utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide, the method is utilized the steel-smelting electric furnace flue dust, ammoniacal liquor or bicarbonate of ammonia etc. are raw material, prepare Nano-class zinc oxide, the zinc oxide productive rate reaches more than 90%.Method steps is simple, and equipment investment is few, and economic benefit is fairly obvious.
The zinc rate (in ZnO) that contains of steel-smelting electric furnace flue dust is generally between 10-35wt%, preferably between 15%-25wt%.Particularly, method of the present invention is suitable for preparing zinc oxide, especially nano level zinc oxide from the steel-smelting electric furnace flue dust that contains the impurity such as Mn, Cu, Cd, Ni.Depend on source, for example, Steel Plant's steel-smelting electric furnace flue dust contains the Mn of 0.1-5wt% (preferred 0.3-3wt%), the Cu of 0.1-6wt% (preferred 0.35-3.5wt%), the Cd of 0.1-4wt% (preferred 0.3-3wt%), and the Ni of 0wt% or 0.001-3wt% (preferred 0.01-2wt% or 0.1-2wt%).
To achieve these goals, the technical solution adopted in the present invention is:
According to the first embodiment of the present invention, provide a kind of method of utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide, it comprises the steps:
1) the steel-smelting electric furnace flue dust of 100 weight parts is placed in to mass concentration and is at least 95% the vitriol oil, the mass ratio of described steel-smelting electric furnace flue dust and the vitriol oil is (0.6～5): 1[preferred 0.8～3): 1, more preferably (1～2.5): 1, as 2:1], fully after reaction, filter, obtain filtrate;
2) in above-mentioned filtrate, add 0.4～4.0 weight part, preferred 0.5～3.5 weight part, more preferably 0.6～3.0 weight part, more preferably 0.7～2.0 weight part, the more preferably PbO of 0.8 weight part～1.2 weight parts
2Powder, and add basic solution, fully stir, allow Fe, Mn generate corresponding precipitation, remove Fe, Mn impurity, reaction formula is:
2Fe
2++PbO
2+4OH
-+H
2O→2Fe(OH)
3↓+PbO↓
Mn
2++PbO
2+2OH
-→PbO↓+MnO
2↓+H
2O
3) by step 2) in Fe, Mn contaminant filter, then add 1.5～10 weight part zinc powders (preferred 2.5～7 weight part zinc, preferred 3～5 weight part zinc powders) in filtrate, remove Pb, Cu, Cd impurity, reaction formula is:
Me
2++ Zn → Me ↓+Zn
2+(Me is Pb, Cu or Cd)
4) filtration step 3) in Pb, Cu, Cd impurity, again to adding q.s (40～200 weight parts for example in filtrate, preferred 50～180 weight parts, as 60,70,80,90,100,120,140,150,160 weight parts) mass concentration be 7%～30% ammoniacal liquor or ammonium bicarbonate soln or the sal volatile of (preferred 9%～25%, as 10%～15%), generate zinc ammonia complex.
Zn
2++(n+2)NH
3·H
2O→[Zn(NH
3)
n](OH)
2+2NH
4 ++(n+1)H
2O。
" q.s " described here refers to that the amount of ammonia or ammonium salt is enough to the whole Zn of complexing
2+Ion.
5) drying step 4) zinc ammonia complex generate nano zine oxide, reaction formula is:
[Zn(NH
3)
n](OH)
2→ZnO↓+n?NH
3↑+H
2O↑。
Preferably, the above dry zinc ammonia complex is spraying drying.
Preferably, after step 3), before step 4), adopt polymeric adsorbent (for example extration resin, think the extration resin success948 of resin company limited as Jiangsu Se Kesai) to remove nickel ion.
Extration resin is adsorbed onto on conventional macroporous polymer carrier (polarity or non-polar support) and is prepared from by extraction agent, for various extracting operations, extract various metals, aspect extraction, wash-out, having particle and two kinds of characteristics of liquid concurrently, have the people that this technology is called to the liquid-solid extraction technology.Chelating and ion exchange resin have than highly selective, but the complicacy that their application in separation are synthesized, expensive and functional group are bonded to difficulty and time-consuming restriction on resin.Although extraction and separation technology is applied in a lot of fields, sometimes easily form third phase, layering difficulty.Consider these deficiencies, extration resin combines solvent extraction and ion-exchange, becomes an important research field in separation science, and its research more and more is subject to people's attention.
In general, the particle diameter of the described nano zine oxide that obtains is 10～80nm, preferred 15～50nm, more preferably 20～40nm, and specific surface area is 35m
2/ g～60m
2/ g, preferred 40m
2/ g～55m
2/ g.
Preferably, described dry zinc ammonia complex is spraying drying.Step 2) basic solution described in is preferably ammoniacal liquor or ammonium bicarbonate soln or sal volatile, its concentration is generally the 10%-20%(weight ratio), steel-smelting electric furnace flue dust with respect to 100 weight parts, its addition is generally 3～25 weight parts, preferred 4～20 weight parts, preferred 5～15 weight parts, as 6～10 weight parts.
By aforesaid method, the present invention's main raw material used is the steel-smelting electric furnace flue dust, by the vitriol oil oxidation of steel-smelting electric furnace flue dust, generate solution of zinc sulfate, then through removing impurities by oxidation, reduction removal of impurities, and repeatedly precipitate, with Se Kesai, think extration resin and remove nickel ion, obtain pure solution of zinc sulfate.The ammoniacal liquor that will prepare again or bicarbonate of ammonia and solution of zinc sulfate reaction generate zinc ammonia complex; The spray-dried generation nano zine oxide of this title complex.The principal reaction formula is as follows:
ZnO+H
2SO
4→ZnSO
4+H
2O
Me+H
2SO
4→ MeSO
4+ H
2O(Me is Fe, Mn, Cu, Pb, Cd, Ni etc.)
Zn
2++NH
4HCO
3+(n+1)NH
3·H
2O→[Zn(NH
3)
n](OH)
2+CO
2+nH
2O+2NH
4 +
[Zn(NH
3)
n](OH)
2→ZnO+nNH
3↑+H
2O↑
Fe in the leaching operation, Mn, Cu, Pb, Cd etc. are also together leached, and when leaching finishes, add PbO
2Except Fe, Mn, reaction formula is:
2Fe
2++PbO
2+4OH
-+H
2O→2Fe(OH)
3↓+PbO↓
Mn
2++PbO
2+2OH
-→PbO↓+MnO
2↓+H
2O
After leaching liquid is filtered, add zinc dust precipitation and remove other impurity.Reaction formula is as follows:
Me
2++ Zn → Me ↓+Zn
2+(Me is Pb, Cu, Cd etc.)
Zn
2++(n+2)NH
3·H
2O→[Zn(NH
3)
n](OH)
2+2NH
4 ++(n+1)H
2O
Compared with prior art, the invention has the beneficial effects as follows: technique of the present invention is simple, and equipment investment is few, and the zinc oxide rate of recovery is high.Gained nano granular of zinc oxide size distribution is even, and median size is at 20～40nm.According to GB/T19589-2004 nano zine oxide, require particle diameter≤100nm, specific surface area>15m
2/ g.So zinc oxide prepared by this technique can meet the requirement of GB/T19589-2004 nano zine oxide.
Method of the present invention is suitable for preparing high-quality zinc oxide, especially nano level zinc oxide from the steel-smelting electric furnace flue dust that contains the impurity such as Mn, Cu, Cd, Ni.Depend on source, for example, Steel Plant's steel-smelting electric furnace flue dust contains the Mn of 0.1-5wt% (preferred 0.3-3wt%), the Cu of 0.1-6wt% (preferred 0.35-3.5wt%), the Cd of 0.1-4wt% (preferred 0.3-3wt%),, and the Ni of 0wt% or 0.001-3wt% (preferred 0.01-2wt% or 0.1-2wt%), in metallic element.
The present invention is further elaborated below in conjunction with embodiment.
Embodiment
Embodiment 1
The steel-smelting electric furnace flue dust that uses in the present embodiment 1 contains the Mn of 0.35wt%, the Cu of 0.43wt%, and the Cd of 0.31wt% and the Ni of 0.25wt%, in metallic element.Remainder is ferriferous oxide, silicon-dioxide, alkalimetal oxide etc.
1, get 1000g and contain zinc rate 15wt% (in ZnO, molecular weight 81.37) the steel-smelting electric furnace flue dust (Mn that contains 0.35wt%, the Cu of 0.43wt%, the Cd of 0.31wt% and the Ni of 0.25wt%), 2:1 adds 95% vitriol oil oxidation in mass ratio, generate solution of zinc sulfate, fully reaction, more than 2 hours, allows flue dust fully dissolve, simultaneously, other metal also generates corresponding vitriol with sulfuric acid reaction, then filters.
2, the PbO that adds 8g in the solution after filtering to step 1
2Powder, and add the ammonium bicarbonate soln (concentration 20wt%) of 40g, fully stir, and makes Fe, and Mn generates corresponding precipitation, with except Fe, the impurity such as Mn.
3, by solution filter, then, to the zinc powder that adds 30g in step 2 solution, fully stir, allow zinc powder and Pb
2+, Cu
2+, Cd
2+Deng reaction, utilize replacement(metathesis)reaction to remove relative substance.
4, after repeatedly precipitating, carry out solid-liquid separation, the solution that step 3 is obtained soaks with (Jiangsu Se Kesai thinks the extration resin success948 of resin company limited), removes nickel ion, obtains pure solution of zinc sulfate.
5, the ammoniacal liquor (molecular weight 17 of ammonia) that is 17wt% to the concentration that adds the 250g for preparing in the solution of step 4 generates zinc ammonia complex with the solution of zinc sulfate reaction.
6, the solution that step 5 is obtained carries out drying (inlet temperature remains on 300 ℃ of left and right, and temperature out remains on 90 ℃ of left and right) with spray-drier, obtains nano zine oxide, and median size is at 20nm, and specific surface area reaches 50m
2/ g, the quality percentage composition of zinc oxide product is 96.6%.
UV-spectrophotometry records foreign matter content: the Mn of<10ppm, the Cu of<8ppm, the Cd of<3ppm and<Ni of 3ppm.
Embodiment 2
The steel-smelting electric furnace flue dust that uses in the present embodiment 2 contains the Mn of 0.43wt%, the Cu of 0.50wt%, the Cd of 0.38wt% and the Ni of 0.0006wt%.Remainder is ferriferous oxide, silicon-dioxide, alkalimetal oxide etc.
1, get the steel-smelting electric furnace flue dust that 1000g contains zinc rate 25wt%, 1:1 adds 98% vitriol oil oxidation in mass ratio, generates solution of zinc sulfate, fully reaction, more than 3 hours, allows flue dust fully dissolve rear filtration, simultaneously, other metal also generates corresponding vitriol with sulfuric acid reaction, then filters.
2, the solution after filtering to step 1 adds the PbO of 12g
2Powder, and add the ammonium bicarbonate soln (concentration 10%) of 50g, fully stir, allow Fe, Mn generate corresponding precipitation, except Fe, the impurity such as Mn.
3, by solution filter, then, to the zinc powder that adds 50g in step 2 solution, fully stir, allow zinc powder and Pb
2+, Cu
2+, Cd
2+Deng reaction, utilize replacement(metathesis)reaction to remove relative substance.
4,, repeatedly after precipitation, after carrying out solid-liquid separation, to adding the 1000g concentration for preparing in step 3, be bicarbonate of ammonia or the sal volatile and solution of zinc sulfate reaction generation zinc ammonia complex of 25wt%.
5, the solution of step 4 being obtained, replace more than 3 times repeatedly with deionized water.Standing 30 minutes, pour out upper water.
6, the zinc ammonia complex solution of step 5 being obtained, carry out spraying drying (inlet temperature remains on 300 ℃ of left and right, and temperature out remains on 90 ℃ of left and right) with spray-drier, obtains nano zine oxide, and median size is at 30nm, and specific surface area reaches 35m
2/ g, the quality percentage composition of zinc oxide is 98.0%.
UV-spectrophotometry records foreign matter content: the Mn of<9ppm, the Cu of<8ppm, the Cd of<3ppm and<Ni of 5ppm.
The content that above-described embodiment is illustrated should be understood to these embodiment only be used to being illustrated more clearly in the present invention, and be not used in, limit the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
Claims (5)
1. a method of utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide, is characterized in that, comprises the steps:
1) the steel-smelting electric furnace flue dust of 100 weight parts is placed in to mass concentration and is at least 95% the vitriol oil, the mass ratio of described steel-smelting electric furnace flue dust and the vitriol oil is (0.6～5): 1, fully after reaction, filter, and obtain filtrate;
2) to the PbO that adds 0.4～4.0 weight part (preferred 0.5 weight part～3.5 weight parts) in above-mentioned filtrate
2Powder, and add basic solution, fully stir, allow Fe, Mn generate corresponding precipitation, remove Fe, Mn impurity, reaction formula is:
2Fe
2++PbO
2+4OH
-+H
2O→2Fe(OH)
3↓+PbO↓
Mn
2++PbO
2+2OH
-→PbO↓+MnO
2↓+H
2O
3) by step 2) in Fe, Mn contaminant filter, then add 1.5～10 weight part zinc powders in filtrate, preferred 2.5～7 weight part zinc powders, remove Pb, Cu, Cd impurity, reaction formula is:
Me
2++ Zn → Me ↓+Zn
2+(Me is Pb, Cu or Cd)
4) filtration step 3) in Pb, Cu, Cd impurity, then, to the mass concentration that adds the 40-200 weight part in filtrate be 7%～30% ammoniacal liquor or ammonium bicarbonate soln or the sal volatile of (preferred 9%～25%, as 15%～25%), generate zinc ammonia complex;
Zn
2++(n+2)NH
3·H
2O→[Zn(NH
3)
n](OH)
2+2NH
4 ++(n+1)H
2O
5) drying step 4) zinc ammonia complex generate nano zine oxide, reaction formula is:
[Zn(NH
3)
n](OH)
2→ZnO↓+n?NH
3↑+H
2O↑。
2. the method for utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide according to claim 1, is characterized in that, described dry zinc ammonia complex is spraying drying.
3. the method for utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide according to claim 1 and 2, is characterized in that, after step 3), before step 4), adopts polymeric adsorbent to remove nickel ion.
4. any one described method of utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide according to claim 1-3, is characterized in that, the particle diameter of described nano zine oxide is 10～80nm, preferred 15～50nm, and specific surface area is 35m
2/ g～60m
2/ g.
5. any one described method of utilizing the steel-smelting electric furnace flue dust to produce nano zine oxide according to claim 1-4, it is characterized in that, step 2) basic solution described in is ammoniacal liquor or ammonium bicarbonate soln or sal volatile, its concentration is generally 10%～20% % by weight, leaching liquid with respect to 100 weight parts, its addition is generally 3～25 weight parts, preferred 4～20 weight parts, for example 5～15 weight parts.
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| CN201310335960.9A CN103395825B (en) | 2012-08-19 | 2013-08-05 | A kind of method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613116A (en) * | 2013-12-09 | 2014-03-05 | 衡阳师范学院 | Method for simultaneously and comprehensively recycling zinc ash and high-arsenic zinc oxide in iron and steel plant |
| CN105347386A (en) * | 2015-11-19 | 2016-02-24 | 北京三聚环保新材料股份有限公司 | Preparation method of nano-zinc oxide |
| CN106219594A (en) * | 2016-08-03 | 2016-12-14 | 王凯 | A kind of preparation method of nano zine oxide |
| CN109879323A (en) * | 2019-02-20 | 2019-06-14 | 武汉科技大学 | It is a kind of to prepare ferritic method using electric furnace dust and mill scale |
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| CN1055766A (en) * | 1991-05-27 | 1991-10-30 | 河北省藁城市化肥厂 | Produce the technology of zinc oxide from containing zinc flue dust |
| CN1210813A (en) * | 1998-07-24 | 1999-03-17 | 山西省稷山县福利化工厂 | Alkaline process for producing active zinc oxide |
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2013
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| CN1055766A (en) * | 1991-05-27 | 1991-10-30 | 河北省藁城市化肥厂 | Produce the technology of zinc oxide from containing zinc flue dust |
| CN1210813A (en) * | 1998-07-24 | 1999-03-17 | 山西省稷山县福利化工厂 | Alkaline process for producing active zinc oxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613116A (en) * | 2013-12-09 | 2014-03-05 | 衡阳师范学院 | Method for simultaneously and comprehensively recycling zinc ash and high-arsenic zinc oxide in iron and steel plant |
| CN103613116B (en) * | 2013-12-09 | 2014-11-05 | 衡阳师范学院 | Method for simultaneously and comprehensively recycling zinc ash and high-arsenic zinc oxide in iron and steel plant |
| CN105347386A (en) * | 2015-11-19 | 2016-02-24 | 北京三聚环保新材料股份有限公司 | Preparation method of nano-zinc oxide |
| CN106219594A (en) * | 2016-08-03 | 2016-12-14 | 王凯 | A kind of preparation method of nano zine oxide |
| CN109879323A (en) * | 2019-02-20 | 2019-06-14 | 武汉科技大学 | It is a kind of to prepare ferritic method using electric furnace dust and mill scale |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103395825B (en) | 2016-02-24 |
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