CN103395825B - A kind of method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide - Google Patents
A kind of method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide Download PDFInfo
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- CN103395825B CN103395825B CN201310335960.9A CN201310335960A CN103395825B CN 103395825 B CN103395825 B CN 103395825B CN 201310335960 A CN201310335960 A CN 201310335960A CN 103395825 B CN103395825 B CN 103395825B
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Abstract
The invention discloses a kind of method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide.In order to solve the problem of existing Steel Plant steel-smelting electric furnace fume recovery difficulty, the described method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide comprises the steps: 1) steel-smelting electric furnace flue dust is placed in the vitriol oil, fully filter after reaction; 2) in leaching liquid, PbO is added
2powder, fully stirs, removing Fe, Mn impurity; 3) filter in backward filtrate and add zinc powder, remove Pb, Cu, Cd impurity; 4) filter in backward filtrate and add ammoniacal liquor or ammonium bicarbonate soln generation zinc ammonia complex; 5) dry zinc ammonia complex generates nano zine oxide.Present invention process is simple, and equipment investment is few, and recovery rate of zinc oxide is high.
Description
Technical field
The present invention relates to a kind of method utilizing 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 is containing zinc 15% ~ 25%.Past China only have more than 50 tons just establish dust arrester installation, but the flue dust collected also does not utilize, and not only jeopardizing environment, is also very large waste to resource.Along with China's hot dip zinc increases considerably, reclaim steel melting furnace flue dust thus realize regenerated zinc produce seem particularly important.
Nano zine oxide is a kind of novel high function fine inorganic product, compared with conventional oxidation zinc, nano zine oxide magnetic, optical, electrical, responsive etc. in there is the incomparable property of general zinc oxide product and novelty teabag.More wide application prospect is shown in rubber, coating, ink, pigment, catalyzer, makeup and medicine and other fields.
CN102826588A discloses the method utilizing steel mill smoke dust ash ammonia method decarburization production high-purity nano-zinc oxide, comprise the following steps: leaching steel plant smoke ash, purification and impurity removal, ammonia still process crystallization and drying and calcining, is characterized in that: leaching steel plant smoke ash ammoniacal liquor-ammonium fluid leaches as leaching agent; 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 0.3-0.5kg Sodium Silicofluoride, obtain leaching liquid after leaching; After leaching, in gained leaching liquid, zinc oxide concentration controls at 50-60g/L, and carry out intensification decarburization, its method is: in every cubic metre of leaching liquid, add 50-60kg white lime, be heated with stirring to 90-98 DEG C, work as CO
2concentration≤0.3mol/L, adds 3-4kg ammonium persulphate in every cubic metre of aforementioned liquids, and adds white lime 10kg/m
3continue stir decarburization and oxidizing reaction occur, 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 process, add tensio-active agent, and add-on is 30-50g tensio-active agent in the liquid after every cubic metre of purification and impurity removal process.
CN102826589A discloses the method utilizing steel plant smoke ash ammonia production high-purity nano-zinc oxide, comprise the following steps: leaching steel plant smoke ash, purification and impurity removal, ammonia still process crystallization and drying and calcining, it is characterized in that: before leaching steel plant smoke ash step, in pending steel plant smoke ash, add white lime obtain compound, and the maintenance mixture moisture content 8-10% that adds water, then carry out admixture activation, the amount of the white lime added, by weight, be the 3-5% of steel plant smoke ash; Steel plant smoke ash ammoniacal liquor-ammonium fluid after admixture activation is leached as leaching agent; 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, adds 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 process, adds ammonium phosphate and tensio-active agent, and add-on is 1-3kg ammonium phosphate in the liquid after every cubic metre of purification and impurity removal process, 10-50g tensio-active agent.
CN102826586A discloses the method utilizing steel plant smoke ash production high-purity nano-zinc oxide, it is characterized in that, comprise the following steps: leaching steel plant smoke ash, purification and impurity removal, ammonia still process crystallization and drying and calcining, it is characterized in that: during leaching steel plant smoke ash, leach as leaching agent with ammoniacal liquor-ammonium fluid; 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 0.3-0.5kg Sodium Silicofluoride, obtain leaching liquid after leaching; Before purification and impurity removal step, carry out pre-ammonia still process, method is: the leaching liquid obtained after leaching is heated to 95-105 DEG C and carries out analysing ammonia, until c (NH in leaching liquid
3)≤3mol/L, then by adding 2-4kg ammonium persulphate in the leaching liquid of every cubic metre and stirring oxidation, the liquid after pre-ammonia still process is carried out solid-liquid separation, solution enters purification and impurity removal step; After purification and impurity removal, carry out refinement treatment, method is: in the liquid after purification and impurity removal process, adds ammonium phosphate and tensio-active agent, and add-on is 1-3kg ammonium phosphate in the liquid after every cubic metre of purification and impurity removal process, 30-50g tensio-active agent.
But the method for prior art seems very difficult for the process of the steel-smelting electric furnace flue dust containing 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 utilizing steel-smelting electric furnace flue dust to produce nano zine oxide, the method utilizes steel-smelting electric furnace flue dust, ammoniacal liquor or bicarbonate of ammonia etc. are raw material, prepare Nano-class zinc oxide, 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 applicable to preparing zinc oxide from the steel-smelting electric furnace flue dust containing impurity such as Mn, Cu, Cd, Ni, especially nano level zinc oxide.Depend on source, such as, 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 utilizing 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 the vitriol oil that mass concentration is at least 95%, the mass ratio of described steel-smelting electric furnace flue dust and the vitriol oil is (0.6 ~ 5): 1 [preferably 0.8 ~ 3): 1, more preferably (1 ~ 2.5): 1, as 2:1], filter after abundant reaction, obtain filtrate;
2) in above-mentioned filtrate, 0.4 ~ 4.0 weight part is added, preferably 0.5 ~ 3.5 weight part, more preferably 0.6 ~ 3.0 weight part, more preferably 0.7 ~ 2.0 weight part, more preferably the PbO of 0.8 weight part ~ 1.2 weight part
2powder, and add basic solution, fully stir, allow Fe, Mn generate corresponding precipitation, removing 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 (preferably 2.5 ~ 7 weight part zinc, preferably 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, q.s (such as 40 ~ 200 weight parts are added again in filtrate, preferably 50 ~ 180 weight parts, as 60,70,80,90,100,120,140,150,160 weight parts) mass concentration be 7% ~ 30% ammoniacal liquor of (preferably 9% ~ 25%, as 10% ~ 15%) or ammonium bicarbonate soln or sal volatile, 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↓+nNH
3↑+H
2O↑。
Preferably, the above dry zinc ammonia complex is spraying dry.
Preferably, after step 3), before step 4), polymeric adsorbent (such as extration resin, as Jiangsu Se Kesai thinks the extration resin success948 of resin company limited) is adopted to remove nickel ion.
Extration resin is adsorbed onto on conventional macroporous polymer carrier (polarity or non-polar support) by extraction agent and is prepared from, for various extracting operation, extract various metal, in extraction, wash-out, have particle and liquid two kinds of features concurrently, have people that this technology is called liquid-solid extraction technology.Chelating and ion exchange resin have comparatively highly selective, but complicacy, high cost and functional group that their application in separation are synthesized are bonded to difficulty on resin and time-consuming restriction.Although extraction and separation technology is applied in a lot of field, sometimes easily form third phase, layering difficulty.Consider that these are not enough, solvent extraction and ion-exchange combine by extration resin, become an important research field in separation science, are more and more subject to people's attention its research.
In general, the particle diameter of the described nano zine oxide obtained is 10 ~ 80nm, preferably 15 ~ 50nm, more preferably 20 ~ 40nm, and specific surface area is 35m
2/ g ~ 60m
2/ g, preferably 40m
2/ g ~ 55m
2/ g.
Preferably, described dry zinc ammonia complex is spraying dry.Step 2) described in basic solution be preferably ammoniacal liquor or ammonium bicarbonate soln or sal volatile, its concentration is generally 10%-20%(weight ratio), relative to the steel-smelting electric furnace flue dust of 100 weight parts, its addition is generally 3 ~ 25 weight parts, preferably 4 ~ 20 weight parts, preferably 5 ~ 15 weight parts, as 6 ~ 10 weight parts.
Above method, the present invention's main raw material used is steel-smelting electric furnace flue dust, is oxidized by the steel-smelting electric furnace flue dust vitriol oil, generate solution of zinc sulfate, then through removing impurities by oxidation, reduction removal of impurities, and repeatedly precipitate, think extration resin removing nickel ion with Se Kesai, obtain pure solution of zinc sulfate.Again the ammoniacal liquor prepared or bicarbonate of ammonia and solution of zinc sulfate are reacted and generate zinc ammonia complex; The spray-dried generation nano zine oxide of this title complex.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↑
In leaching operation, Fe, Mn, Cu, Pb, Cd etc. are also together leached, at the end of leaching, 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
Add zinc dust precipitation after being filtered by leaching liquid 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: present invention process is simple, and equipment investment is few, and recovery rate of zinc oxide is high.Gained nano granular of zinc oxide even particle size distribution, median size is at 20 ~ 40nm.Particle diameter≤100nm, specific surface area >15m is required according to GB/T19589-2004 nano zine oxide
2/ g.Therefore the zinc oxide that prepared by this technique can meet the requirement of GB/T19589-2004 nano zine oxide.
Method of the present invention is applicable to preparing high-quality zinc oxide from the steel-smelting electric furnace flue dust containing impurity such as Mn, Cu, Cd, Ni, especially nano level zinc oxide.Depend on source, such as, 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%), with elemental metal.
Below in conjunction with embodiment, the present invention is further elaborated.
Embodiment
Embodiment 1
The steel-smelting electric furnace flue dust used in the present embodiment 1 contains the Mn of 0.35wt%, and the Cu of 0.43wt%, the Ni of Cd and 0.25wt% of 0.31wt%, with elemental metal.Remainder is ferriferous oxide, silicon-dioxide, alkalimetal oxide etc.
1,1000g is got containing zinc rate 15wt% (in ZnO, molecular weight 81.37) the steel-smelting electric furnace flue dust (Mn containing 0.35wt%, the Ni of Cd and 0.25wt% of the Cu of 0.43wt%, 0.31wt%), 2:1 adds the vitriol oil oxidation of 95% in mass ratio, generate solution of zinc sulfate, abundant reaction more than 2 hours, allows flue dust fully dissolve, simultaneously, other metal also generates corresponding vitriol to sulfuric acid reaction, then filters.
2, the PbO of 8g is added in the solution after filtering to step 1
2powder, and the ammonium bicarbonate soln (concentration 20wt%) adding 40g, fully stir, make Fe, and Mn generates corresponding precipitation, to remove the impurity such as Fe, Mn.
3, solution is filtered, then in step 2 solution, add the zinc powder of 30g, fully stir, allow zinc powder and Pb
2+, Cu
2+, Cd
2+deng reaction, replacement(metathesis)reaction is utilized to remove relative substance.
4, after repeatedly precipitating, carry out solid-liquid separation, solution step 3 obtained soaks with (Jiangsu Se Kesai thinks the extration resin success948 of resin company limited), and removing nickel ion, obtains pure solution of zinc sulfate.
5, to be the ammoniacal liquor of 17wt% (molecular weight 17 of ammonia) with solution of zinc sulfate react the concentration adding the 250g prepared in the solution of step 4 generates zinc ammonia complex.
6, solution spray-drier step 5 obtained carries out drying (inlet temperature remains on about 300 DEG C, and temperature out remains on about 90 DEG C), and obtain nano zine oxide, median size is at 20nm, and specific surface area reaches 50m
2/ g, the mass percentage of zinc oxide product is 96.6%.
UV-spectrophotometry records foreign matter content: the Ni of Cd and <3ppm of the Cu of the Mn of <10ppm, <8ppm, <3ppm.
Embodiment 2
The steel-smelting electric furnace flue dust used in the present embodiment 2 contains the Mn of 0.43wt%, the Cu of 0.50wt%, the Ni of Cd and 0.0006wt% of 0.38wt%.Remainder is ferriferous oxide, silicon-dioxide, alkalimetal oxide etc.
1, get the steel-smelting electric furnace flue dust of 1000g containing zinc rate 25wt%, 1:1 adds the vitriol oil oxidation of 98% in mass ratio, generates solution of zinc sulfate, abundant reaction more than 3 hours, allows flue dust fully dissolve rear filtration, simultaneously, other metal also generates corresponding vitriol to sulfuric acid reaction, then filters.
2, the solution after filtering to step 1 adds the PbO of 12g
2powder, and the ammonium bicarbonate soln (concentration 10%) adding 50g, fully stir, and allows Fe, Mn generate corresponding precipitation, except impurity such as Fe, Mn.
3, solution is filtered, then in step 2 solution, add the zinc powder of 50g, fully stir, allow zinc powder and Pb
2+, Cu
2+, Cd
2+deng reaction, replacement(metathesis)reaction is utilized to remove relative substance.
4, repeatedly after precipitation, after carrying out solid-liquid separation, in step 3, add bicarbonate of ammonia or sal volatile that the 1000g concentration prepared is 25wt% and solution of zinc sulfate react and generate zinc ammonia complex.
5, solution step 4 obtained, replaces more than 3 times repeatedly with deionized water.Leave standstill 30 minutes, pour out upper water.
6, zinc ammonia complex solution step 5 obtained, carry out spraying dry (inlet temperature remains on about 300 DEG C, and temperature out remains on about 90 DEG C) with spray-drier, obtain nano zine oxide, median size is at 30nm, and specific surface area reaches 35m
2/ g, the mass percentage of zinc oxide is 98.0%.
UV-spectrophotometry records foreign matter content: the Ni of Cd and <5ppm of the Cu of the Mn of <9ppm, <8ppm, <3ppm.
The content that above-described embodiment is illustrated should be understood to these embodiments only for being illustrated more clearly in the present invention, and be not used in and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Claims (9)
1. utilize steel-smelting electric furnace flue dust to produce a method for nano zine oxide, it is characterized in that, comprise the steps:
1) the steel-smelting electric furnace flue dust of 100 weight parts is placed in the vitriol oil that mass concentration is at least 95%, the mass ratio of described steel-smelting electric furnace flue dust and the vitriol oil is (0.6 ~ 5): 1, fully filters after reaction, obtains filtrate;
2) in above-mentioned filtrate, add the PbO of 0.4 ~ 4.0 weight part
2powder, and add basic solution, fully stir, allow Fe, Mn generate corresponding precipitation, removing 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, remove Pb, Cu, Cd impurity, reaction formula is:
Me
2++ Zn → Me ↓+Zn
2+, wherein Me is Pb, Cu or Cd;
4) filtration step 3) in Pb, Cu, Cd impurity, then the mass concentration adding 40-200 weight part in filtrate is ammoniacal liquor or ammonium bicarbonate soln or the sal volatile of 7% ~ 30%, generates zinc ammonia complex:
Zn
2++6NH
3·H
2O——→[Zn(NH
3)
4]
2++2OH
-+2NH
4 ++4H
2O
5) drying step 4) zinc ammonia complex generate nano zine oxide, reaction formula is:
[Zn(NH
3)
4]
2++2OH
-→ZnO+4NH
3↑+H
2O↑。
2. the steel-smelting electric furnace flue dust that utilizes according to claim 1 produces the method for nano zine oxide, it is characterized in that, in step 2) in filtrate, add the PbO of 0.5 weight part ~ 3.5 weight part
2powder.
3. the method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide according to claim 1, is characterized in that, in step 3) in, then in filtrate, add 2.5 ~ 7 weight part zinc powders.
4. the method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide according to claim 1, it is characterized in that, in step 4) in, then the mass concentration adding 40-200 weight part in filtrate is ammoniacal liquor or ammonium bicarbonate soln or the sal volatile of 15% ~ 25%.
5. the method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide according to claim 1, it is characterized in that, described dry zinc ammonia complex is spraying dry.
6. produce the method for nano zine oxide according to the steel-smelting electric furnace flue dust that utilizes in claim 1-3 described in any one, it is characterized in that, in step 3) after, step 4) before, adopt polymeric adsorbent removing nickel ion.
7. produce the method for nano zine oxide according to the steel-smelting electric furnace flue dust that utilizes in claim 1-3 described in any one, it is characterized in that, the particle diameter of described nano zine oxide is 10 ~ 80nm, and specific surface area is 35m
2/ g ~ 60m
2/ g.
8. produce the method for nano zine oxide according to the steel-smelting electric furnace flue dust that utilizes in claim 1-3 described in any one, it is characterized in that, step 2) described in basic solution be ammoniacal liquor or ammonium bicarbonate soln or sal volatile, its concentration is 10 ~ 20 % by weight, relative to the leaching liquid of 100 weight parts, its addition is 3 ~ 25 weight parts.
9. the steel-smelting electric furnace flue dust that utilizes according to claim 8 produces the method for nano zine oxide, it is characterized in that, relative to the leaching liquid of 100 weight parts, ammoniacal liquor or ammonium bicarbonate soln or sal volatile addition are 5 ~ 15 weight parts.
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| 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 |
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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 |
-
2013
- 2013-08-05 CN CN201310335960.9A patent/CN103395825B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Title |
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| 用含锌烟尘制备活性氧化锌的工艺研究;李海普等;《湖南化工》;19980831;第28卷(第4期);第20-22页 * |
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