CN103937914A - Method for total resource utilization of LF furnace refining slag - Google Patents

Method for total resource utilization of LF furnace refining slag Download PDF

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CN103937914A
CN103937914A CN201410152388.7A CN201410152388A CN103937914A CN 103937914 A CN103937914 A CN 103937914A CN 201410152388 A CN201410152388 A CN 201410152388A CN 103937914 A CN103937914 A CN 103937914A
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slag
refining slag
refining
mgo
sio
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CN103937914B (en
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徐国平
黄毅
程慧高
万迎峰
杨巍
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Sinosteel Wuhan Safety & Environmental Protection Research Institute Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

Abstract

The invention relates to a method for total resource utilization of LF (Ladle Furnace) refining slag. The method comprises the following steps: preprocessing LF refining slag, so that the refining slag is divided into high aluminum slag, high silicon slag and silicon aluminum slag, mixing any two of the three classes of refining slag at a mass ratio, and preparing slurry with water; performing a carbonation reaction, NaOH alkali dissolution to extract silicon and aluminum, filtration as well as an aging reaction and a crystallization reaction, so as to separate main components, namely CaO, MgO, Si2O3 and Al2O3 in the refining slag; meanwhile, removing S in the slag, making the CaO and MgO components into a steel making or sintering solvent, and making the Si2O3 and Al2O3 components into 4A zeolite. The method disclosed by the invention can be used for realizing total resource utilization of the LF refining slag; moreover, the method is simple in process and is capable of recycling waste, and the method has excellent economical and environmental benefits.

Description

A kind of method of LF furnace refining slag full dose recycling
Technical field
The invention belongs to slag comprehensive utilization technical field, particularly a kind of method of LF furnace refining slag full dose recycling.
Background technology
Slag is the waste residue producing in steelmaking process, can be divided into carbon steel slag and stainless steel slag according to steel grade; Can be divided into pre-treatment slag, bessemer furnace slag, electric furnace slag, refining slag and residual casting slag China's output of steel in 2010 according to process for making and reach 6.267 hundred million tons, produce slag per year and will reach 9,000 ten thousand tons, and the comprehensive utilization ratio of China's slag be only 22%.Refining slag is the one of slag, and output accounts for 5% of slag ultimate production.At present, the utilization that each steel is looked forward to refining slag is mainly utilized as master with internal recycling, comprises that being back to use refining furnace continues refining, is back to use converter as fusing assistant.Compacting balling-up after as Chinese patent CN101463406, LF furnace refining slag being coordinated with iron fine powder, is back to use converter as steel-making flux, obtains reasonable effect.Chinese patent CN103045778 makes refining slag by LF stove steel scrap cinder inclusion slag after naturally cooling, magnetic separation, fragmentation, screening, be conducive to improve ladle slag adsorbent silicate and be mingled with ability, reduce molten steel oxidation, reduce converter steel iron charge and alloy consumption, further improve steel quality.Chinese patent CN103276201 discloses a kind of circulation utilization method of carbon steel LF refining slag, by refining slag pressure ball, can replace pre-melted slag to use after maintenance.Easily cause molten steel to pollute because contain the impurity such as S in refining slag, therefore limited the amount of its reuse in metallurgical process.Chinese patent CN101717843 sloughs the S of refining slag by the method for roasting, but this method cost is high, and can only slough the S in CaS, and cannot slough the S being solid-solubilized in calcium aluminate and calcium aluminate.Because the amount of the metallurgical reuse of refining slag is limited, therefore most refining slag still saves as master with heap in iron and steel enterprise, or simple and converter slag mixes and be used, and the utility value of refining slag is not given full play to.
Except metallurgical reuse, Chinese patent CN101402460 and CN101259969 disclose respectively with acidleach and Na 2cO 3alkali dissolution method extracts the method for Al in refining slag.Acidleach method acid consumption is large, and aluminium solubility rate is low, and Na 2cO 3alkali dissolution method again may be by the Si stripping in slag, thereby makes the Al obtaining 2o 3product contains Si impurity, and the S in slag also cannot remove.And these two kinds of methods for be only high Al refining slag, and be not suitable for the refining slag that Si content is high.
Summary of the invention
The object of the invention is the utility value existing for above refining slag comprehensive utilization and utilize approach problem, a kind of method of LF furnace refining slag full dose recycling is provided.
Technical solution of the present invention is: mix refining slag by a certain percentage (1) with water, utilizes Calucium Silicate powder, calcium aluminate, calcium oxide, the magnesium oxide composition in refining slag and has the CO of certain pressure 2gas generation gas-liquid-solid reaction, can generate calcium carbonate fast, magnesiumcarbonate, and aluminium hydroxide and silicic acid, the CaS in slag generates H with the S reaction being solid-solubilized in Calucium Silicate powder and calcium aluminate simultaneously 2s is discharged in air, H 2s exhaust gas utilization alkali liquor absorption.
(2) utilize aluminium hydroxide and silicic acid to be dissolved in the feature of highly basic, in refining slag after carbonic acid, add NaOH, aluminium hydroxide and silicic acid are extracted in the middle of liquid phase, the main component of solid residue is calcium carbonate and magnesiumcarbonate, similar with Wingdale composition to the raw material rhombspar of steel-making and staflux, and objectionable constituent S obviously reduces in slag, by recycling as steel-making or staflux in steel mill inside after washing and being dried, the waste lye that washing produces can be for H 2s waste gas absorption.
(3) main component in the molten rear liquid phase of alkali is water glass and sodium metaaluminate, is the raw material of preparing zeolite, and 4A zeolite (chemical formula is Na 12al 12si 12o 4827H 2o), preparation technology is simple, can make the auxiliary agent of free phosphate detergent, can be widely used as dry, the dewatered clean of gas and liquid etc. in oil and other industry, also can be used as catalyzer and water-softening chemicals.
From the chemical formula of 4A zeolite, its Si/Al mol ratio is 1, just requires the Si/Al mol ratio in the molten rear liquid phase of alkali approach or equal 1.
Same iron and steel enterprise is because of the difference of steel grade, the difference of raw material, the difference of technique, the SiO of refining slag 2, Al 2o 3content is difference to some extent, as the SiO of certain three kinds of LF furnace refining slag of steel mill 2, Al 2o 3mass content is respectively 23.54%, 12.10; 28.34%, 6.10%; 37.65%, 4.35%.Therefore, the key point of present method is to formulate the appropriate proportioning of different refining slags, makes silica alumina ratio in the molten rear liquid phase of alkali reach the requirement of preparing 4A zeolite, and the multiple refining slag that so also same steel can be looked forward to carries out recycling simultaneously.Based on this, the present invention by LF furnace refining slag according to SiO in slag 2and Al 2o 3the difference of content is divided into high white residue, high alumina slag and aluminium white residue, and has formulated the ratio range that various slags are suitable.
Concrete steps of the present invention are as follows: the pre-treatment of (1) refining slag: LF furnace refining slag is carried out to fragmentation, selects iron, is ground to the pre-treatment below 0.1mm.
(2) classification of refining slag: by pretreated refining slag according to SiO 2and Al 2o 3content is divided into high alumina slag, high white residue and sial slag.The chemical composition scope of high alumina slag is: 35% ~ 60%CaO, 2% ~ 15%SiO 2, 20% ~ 35% Al 2o 3, 2% ~ 5%MgO, 0.5% ~ 3% Fe 2o 3, 0.3 ~ 5% SO 3, the chemical composition scope of high white residue is 35% ~ 60%CaO, 20% ~ 40%SiO 2, 1% ~ 5% Al 2o 3, 2% ~ 5%MgO, 0.5% ~ 3% Fe 2o 3, 0.3 ~ 5% SO 3, the chemical composition scope of sial slag is 35% ~ 60%CaO, 10% ~ 20%SiO 2, 10% ~ 20% Al 2o 3, 2% ~ 10%MgO, 0.5% ~ 3% Fe 2o 3, 0.3 ~ 5% SO 3.
(3) batching of refining slag and mixing: take wherein two kinds of step (2) described high alumina slag, high white residue or sial slag according to certain mass ratio and prepare burden, then at mixer, two kinds of refining slags are fully mixed.While using high alumina slag and high white residue to prepare burden, the preferred mass of two kinds of slags is 0.7 ~ 1.2 than scope, and while using high alumina slag or high white residue and sial slag to prepare burden, the preferred mass of two kinds of slags is 0.05 ~ 0.3 than scope.
(4) the absorption processing of the carbonating of refining slag and slag medium sulphide content: be that 1:1 ~ 1:10 mix with water by solid-to-liquid ratio by mixing sufficient refining slag in step (3), and stir, make refining slag suspension, then pass into CO in suspension 2gas, CO 2gas source is industrial gaseous waste or manually production, and volumetric concentration is 50% ~ 100%, CO 2gas preferred pressure is 0.2 ~ 5 normal atmosphere, and the time of passing into is 30 ~ 90min, and suspension temperature is preferably 65 DEG C ~ 90 DEG C, and the S in slag is with H 2s form is disengaged, and the NaOH alkali lye that is 1% ~ 5% by concentration is to H 2s absorbs processing.
(5) the molten Si of carrying of the alkali of refining slag, Al: add NaOH in the slag after step (4) carbonating, the add-on of NaOH is 20% ~ 50% of refining slag, afterwards suspension is fully stirred under 60 ~ 90 DEG C of conditions to 30 ~ 120min, finally filtration or centrifugal, is separated solid-liquid two.
(6) steel-making or the preparation of staflux: the solid residue water obtaining in step (5) is fully washed until neutral, and can be as steel-making or staflux after drying.Washing water are retained for the H described in step (4) 2s absorbs.
(7) 4A zeolite preparation: by the liquid phase obtaining in step (5) for the preparation of zeolite.Be after ageing 1 ~ 2h, to be crystallization 4 ~ 8h under 85 ~ 95 DEG C of conditions in temperature under 60 ~ 70 DEG C of conditions by liquid phase in temperature, finally filter, wash and obtain 4A zeolite.
The invention has the beneficial effects as follows: the present invention utilizes refining slag to prepare steel-making or staflux and 4A zeolite, remove the S in refining slag, take full advantage of the valuable constituent in refining slag, realized the full dose utilization of refining slag, greatly improved the utilization ratio of refining slag and utilized benefit; And can realize the CO of iron and steel enterprise 2reduce discharging.Technique of the present invention is simple, can realize waste recycling, has good economic benefit and environmental benefit.
Brief description of the drawings
Fig. 1 is the process flow sheet of carbonating refining slag preparation steel-making flux of the present invention and zeolite.
Embodiment
Below in conjunction with several specific exampless, the present invention is further understood in exemplary illustration and help.
embodiment 1
Certain two kinds of LF furnace refining slag of steel enterprise, after fragmentation, magnetic separation and grinding pre-treatment, chemical composition is respectively (1) CaO54.62%, SiO 212.10%, Al 2o 323.54%, MgO4.48%, Fe 2o 31.74%, SO 32.11%; (2) CaO57.48%, SiO 227.73%, Al 2o 31.76%, MgO7.02%, Fe 2o 30.19%, SO 30.87%; Two kinds of refining slags are mixed and become slurries with water by 1:4 proportional arrangement by the mass ratio of 0.85:1, and 0.3MPa pressure, passes into CO under 85 DEG C of conditions 2gas, CO 2void fraction 95%, absorbs H with 2%NaOH waste lye in venting process 2s waste gas, after 60min, stops ventilation.In slurries, add NaOH, NaOH add-on is 30% of refining slag dry weight, and suspension is fully stirred after 60min at 65 DEG C, and slurries are filtered, and filter cake fully washs post-drying, and washing waste lye is used for absorbing H 2s waste gas, CaCO in slag after drying 3and MgCO 3content is greater than 95%, Fe 2o 3content is less than 1%, S content and is less than 0.1%, can be used as making steel flux.Now, the H in liquid phase 2o/Na 2o mol ratio is 65, SiO 2/ Al 2o 3mol ratio is 1.99, Na 2o/SiO 2mol ratio is 0.98, and liquid phase is placed in to 75 DEG C of environment ageing 2h, then in 95 DEG C of environment after crystallization 8h, filtering separation, washing leaching cake, to neutral, obtains 4A zeolite after drying.
embodiment 2
Certain two kinds of LF furnace refining slag of steel enterprise, after fragmentation, magnetic separation and grinding pre-treatment, chemical composition is respectively (1) CaO39.82%, SiO 237.65%, Al 2o 34.35%, MgO10.59%, Fe 2o 31.62%, SO 30.49%; (2) CaO52.86%, SiO 25.71%, Al 2o 323.36%, MgO4.88%, Fe 2o 33.53%, SO 30.87%; Two kinds of refining slags are mixed and become slurries with water by 1:4.6 proportional arrangement by the mass ratio of 1.13:1, and 1MPa pressure, passes into CO under 80 DEG C of conditions 2gas, CO 2void fraction 90%, absorbs H with waste lye in venting process 2s waste gas, after 30min, stops ventilation.In slurries, add NaOH, NaOH add-on is 34% of refining slag dry weight, and suspension is fully stirred after 60min at 70 DEG C, and slurries are filtered, and filter cake fully washs post-drying, and washing waste lye is used for absorbing H 2s waste gas, CaCO in slag after drying 3and MgCO 3content is greater than 90%, Fe 2o 3content is less than 2%, S content and is less than 0.05%, can be transported to sintering plant as staflux.Now, the H in liquid phase 2o/Na 2o mol ratio is 60, SiO 2/ Al 2o 3mol ratio is 1.98, Na 2o/SiO 2mol ratio is 1.08, and liquid phase is placed in to 70 DEG C of environment ageing 2h, then in 95 DEG C of environment after crystallization 6h, filtering separation, washing leaching cake, to neutral, obtains 4A zeolite after drying.
embodiment 3
Certain two kinds of LF furnace refining slag of steel enterprise, after fragmentation, magnetic separation and grinding pre-treatment, chemical composition is respectively (1) CaO52.86%, SiO 25.71%, Al 2o 323.36%, MgO4.88%, Fe 2o 32.53%, SO 30.87%; (2) CaO53.02%, SiO 219.78%, Al 2o 313.14%, MgO3.58%, Fe 2o 31.46%, SO 31.61%; Two kinds of refining slags are mixed and become slurries with water by 1:3 proportional arrangement by the mass ratio of 0.25:1, and 0.2MPa pressure, passes into CO under 85 DEG C of conditions 2gas, CO 2void fraction 60%, absorbs H with waste lye in venting process 2s waste gas, after 80min, stops ventilation.In slurries, add NaOH, NaOH add-on is 24% of refining slag dry weight, and suspension is fully stirred after 40min at 80 DEG C, and slurries are filtered, and filter cake fully washs post-drying, and washing waste lye is used for absorbing H 2s waste gas, CaCO in slag after drying 3and MgCO 3content is greater than 95%, Fe 2o 3content is less than 2%, S content and is less than 0.05%, can be transported to steelworks as steel-making flux.Now, the H in liquid phase 2o/Na 2o mol ratio is 58, SiO 2/ Al 2o 3mol ratio is 2.01, Na 2o/SiO 2mol ratio is 1.02, and liquid phase is placed in to 80 DEG C of environment ageing 2h, then in 95 DEG C of environment after crystallization 4h, filtering separation, washing leaching cake, to neutral, obtains 4A zeolite after drying.
embodiment 4
Certain two kinds of LF furnace refining slag of steel enterprise, after fragmentation, magnetic separation and grinding pre-treatment, chemical composition is respectively (1) CaO39.82%, SiO 237.65%, Al 2o 34.35%, MgO10.59%, Fe 2o 31.62%, SO 30.49%; (2) CaO55.14%, SiO 212.78%, Al 2o 316.14%, MgO2.02%, Fe 2o 31.15%, SO 31.13%; Two kinds of refining slags are mixed and become slurries with water by 1:2 proportional arrangement by the mass ratio of 0.14:1, and 0.5MPa pressure, passes into CO under 85 DEG C of conditions 2gas, CO 2void fraction 99%, absorbs H with waste lye in venting process 2s waste gas, after 40min, stops ventilation.In slurries, add NaOH, NaOH add-on is 21% of refining slag dry weight, and suspension is fully stirred after 35min at 85 DEG C, and slurries are filtered, and filter cake fully washs post-drying, and washing waste lye is used for absorbing H 2s waste gas, CaCO in slag after drying 3and MgCO 3content is greater than 95%, Fe 2o 3content is less than 1%, S content and is less than 0.03%, can be transported to steelworks as steel-making flux.Now, the H in liquid phase 2o/Na 2o mol ratio is 55, SiO 2/ Al 2o 3mol ratio is 2.02, Na 2o/SiO 2mol ratio is 1.01, and liquid phase is placed in to 85 DEG C of environment ageing 4h, then in 90 DEG C of environment after crystallization 4h, filtering separation, washing leaching cake, to neutral, obtains 4A zeolite after drying.

Claims (7)

1. the method for a LF furnace refining slag full dose recycling, it is characterized in that after the pre-treatment of LF furnace refining slag, be divided into high alumina slag, high white residue and sial slag, by in three class refining slags any two kinds in mass ratio mix after and water make slurries, by molten silicon and aluminium, filtration and ageing, the crystallization carried of carbonation reaction, NaOH alkali, realize main component CaO, MgO and Si in refining slag afterwards 2o 3, Al 2o 3component separating is sloughed the S in slag simultaneously, and CaO, MgO composition are made to steel-making or staflux, Si 2o 3, Al 2o 3composition is made 4A zeolite.
2. according to the method for a kind of LF furnace refining slag full dose recycling described in right 1, its characterization step is as follows:
(1) pre-treatment of refining slag: LF furnace refining slag is carried out to fragmentation, selects iron, is ground to below 0.1mm;
(2) classification of refining slag: by pretreated refining slag according to SiO 2and Al 2o 3content is divided into high alumina slag, high white residue and sial slag;
(3) batching of refining slag and mixing: take wherein two kinds of step (2) described high alumina slag, high white residue or sial slag according to mass ratio and prepare burden, then at mixer, two kinds of refining slags are fully mixed;
(4) the absorption processing of the carbonating of refining slag and slag medium sulphide content: it is that 1:1 ~ 1:10 mixes with water by solid-to-liquid ratio that step (3) is mixed to sufficient refining slag, and stirs, and makes refining slag suspension, then passes into CO in suspension 2gas, volumetric concentration is 50% ~ 100%, CO 2gas preferred pressure is 0.2 ~ 5 normal atmosphere, and the time of passing into is 30 ~ 90min, and suspension temperature is preferably 65 DEG C ~ 90 DEG C, and the S in slag is with H 2s form is disengaged, and the NaOH alkali lye that is 1% ~ 5% by concentration is to H 2s absorbs processing;
(5) the molten Si of carrying of the alkali of refining slag, Al: add NaOH in the slag after step (4) carbonating, the add-on of NaOH is 20% ~ 50% of refining slag, afterwards suspension is fully stirred under 60 ~ 90 DEG C of conditions to 30 ~ 120min, finally filtration or centrifugal, is separated solid-liquid two;
(6) steel-making or the preparation of staflux: the solid residue water obtaining in step (5) is fully washed until neutral, and can be as steel-making or staflux after drying; Washing water are retained for the H described in step (4) 2s absorbs;
(7) 4A zeolite preparation: for the preparation of zeolite, be to be crystallization 4 ~ 8h under 85 ~ 95 DEG C of conditions in temperature after ageing 1 ~ 2h under 60 ~ 70 DEG C of conditions by liquid phase in temperature by the liquid phase obtaining in step (5), finally filter, wash and obtain 4A zeolite.
3. according to the method for a kind of LF furnace refining slag full dose recycling described in right 2, it is characterized in that the chemical composition scope of high alumina slag is: 35% ~ 60%CaO, 2% ~ 15%SiO 2, 20% ~ 35% Al 2o 3, 2% ~ 5%MgO, 0.5% ~ 3% Fe 2o 3, 0.3 ~ 5% SO 3.
4. according to the method for a kind of LF furnace refining slag full dose recycling described in right 2, the chemical composition scope that it is characterized in that high white residue is 35% ~ 60%CaO, 20% ~ 40%SiO 2, 1% ~ 5% Al 2o 3, 2% ~ 5%MgO, 0.5% ~ 3% Fe 2o 3, 0.3 ~ 5% SO 3.
5. according to the method for a kind of LF furnace refining slag full dose recycling described in right 2, the chemical composition scope that it is characterized in that sial slag is 35% ~ 60%CaO, 10% ~ 20%SiO 2, 10% ~ 20% Al 2o 3, 2% ~ 10%MgO, 0.5% ~ 3% Fe 2o 3, 0.3 ~ 5% SO 3.
6. according to the method for a kind of LF furnace refining slag full dose recycling described in right 2, while it is characterized in that using high alumina slag and high white residue to prepare burden, the preferred mass of two kinds of slags is 0.7 ~ 1.2 than scope.
7. according to the method for a kind of LF furnace refining slag full dose recycling described in right 2, while it is characterized in that using high alumina slag or high white residue and sial slag to prepare burden, the preferred mass of two kinds of slags is 0.05 ~ 0.3 than scope.
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