CN106367154A - Method for preparing iron-base inhibitor from converter steel slag and application thereof - Google Patents
Method for preparing iron-base inhibitor from converter steel slag and application thereof Download PDFInfo
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- CN106367154A CN106367154A CN201610877363.2A CN201610877363A CN106367154A CN 106367154 A CN106367154 A CN 106367154A CN 201610877363 A CN201610877363 A CN 201610877363A CN 106367154 A CN106367154 A CN 106367154A
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- inhibitor
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L9/00—Treating solid fuels to improve their combustion
- C10L9/10—Treating solid fuels to improve their combustion by using additives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2230/00—Function and purpose of a components of a fuel or the composition as a whole
- C10L2230/08—Inhibitors
Abstract
The invention discloses a method for preparing an iron-base inhibitor mainly from a metallurgical converter steel slag extract and application of the inhibitor in inhibiting coal NO emission, belonging to the technical fields of solid waste high-added-value utilization and pollution control. The method comprises the following steps: decomposing complex components in the converter slag by acidification-precipitation dissolution, firstly removing Ca, using the Fe, Al and other components capable of inhibiting NO generation, which exist in an acid hydrolysis solution in the form of ions, as element sources for preparing the NO inhibitor, and finally, adding hydrochloric acid to precipitate, thereby obtaining the target product. The method overcomes the limit of single dependence on chemical reagents and non-renewable resources in the prior art, fully utilizes the valuable components in the metallurgical solid waste, and provides a new way for high-added-value utilization of iron-containing metallurgical steel slag on the premise of lowering the preparation cost and reducing the oxynitride emission.
Description
Technical field
The invention belongs to solid waste comprehensive utilization and pollution control technology field are and in particular to one kind is based on converter slag
The method wanting the coal-fired nitrogen oxides inhibitor of raw material preparation.
Background technology
China be discharged into every year the 60% of NO_x in Air Environment (nox) derive from coal-fired it can be seen that, nox is coal
The nox of one of important pollutant producing in combustion process, wherein station boiler discharge accounts for more than the 40% of coal fire discharged nox,
In the coal-fired nox producing, more than 90% is no.Therefore research and develop and effectively suppress the additive of coal-fired no discharge to have far-reaching significance.
Being based on experimental study and business-like fire coal nitrogen oxides inhibitor at present both at home and abroad is all with chemical reagent or one
Secondary mineral resources are prepared for raw material, Zhejiang University's heat energy et al. by carbide slag, calcite, aluminium base mineral effective ingredient
(mainly Cabase compound) is blended, and this additive shows good denitration in the soil industry test of chain stove
Effect.Renmin University of China's coal chemistry institute research shows that the iron-based adulterating and calcio can significantly be catalyzed coal tar and reduce the anti-of no
Should, and the catalytic action of doped iron base is better than calcio.The research of energy and power engireering institute of Xi'an Communications University finds iron content
Compound (fecl3,fecl2And fe2o3) all can affect the emission equivalent of coal-fired nitrogen oxides, fec13Both played the work of catalyst
With playing the effect of absorbent simultaneously again.fecl3Catalytic action shows the apparent activation energy reducing no reaction of formation, makes no
Can quickly form in lower temperature, accelerate the speed of no reaction of formation；Additionally, fecl2To no emission performance in flue gas
Impact and fecl3Similar, but impact effect compares fecl3Slightly poor, fe2o3Also the volumetric concentration of no in flue gas can be reduced, abroad
The research of expert ohtsaka et al. also indicates that: the iron containing compoundses in the iron salt filling in de-ash coal or coal mineral itself, energy
In catalysis coal, part nitrogen is converted into n in pyrolytic process2.
Through retrieval, with the technology of the standby fire coal nitrogen oxides inhibitor of prepared from steel slag in iron containing metallurgical solid waste, there is not been reported.Smelting
Golden slag is one of main garbage of steel and iron industry, does not contain only substantial amounts of fe (40%～90%) outward, also contain ca, al, si,
Mg etc. and multiple a small amount of, micro transition metal (p, mn, cr, ti, v etc.), are a kind of valuable metallurgy secondary resources,
But so far, being confined to the utilization practice of converter slag more civil engineering and a small amount of return Ferrous Metallurgy process as sintering,
Slag former.The former belongs to the low value-added Land use models of slag；The latter belongs to the higher Land use models of added value, but p in invar slag
Measure higher and be restricted.Therefore, for a dual difficult problem for current China metallurgical steel slag solid waste discharge and Coal-smoke Air Pollution, from
The angle of " with pollution treatment of giving up " is set out, and finds key component fe, al, mg in the solid waste " metallurgical steel slag " of metallurgical industry discharge
And micro transition metal belongs to the component of coal-fired fe base nitrogen oxides inhibitor, due to playing catalysis to coal burning
Agent acts on, so there is reciprocal action to the component easily generating nitrogen oxides in coal, reaches the effect of collaborative suppression no discharge,
And this solid waste system is applied to administers the research in coal-fired discharged nitrous oxides field and yet there are no and report for work.Therefore, metallurgical steel slag
Possesses the basis as coal-fired nitrogen oxides inhibitor.
Content of the invention
For overcoming the deficiencies in the prior art, the technical problem to be solved in the invention is to propose one kind with metallurgical converter slag
The method that extract prepares iron-based inhibitor for primary raw material, to overcoming tradition fire coal nitrogen oxides inhibitor raw material to rely on one
Secondary resource and the limitation of chemical reagent, provide new way for metallurgical steel slag high value added utilization, also for controlling coal-fired nitrogen oxides
Discharge provides technical strategies.
In order to solve above technical problem, present invention one kind prepares iron-based with metallurgical converter slag extract for primary raw material
The method of inhibitor, specifically comprises the following steps that
(1) first ball milling is carried out to metallurgical converter slag, make sample granularity reach below 200 mesh, then this slag is added
Sulphuric acid adjusts ph value to 2～4, stirs 30min, makes the ca particle in solution with caso4The form of precipitation separates out, sucking filtration, washing
Filter cake 2 times, sucking filtration to filtrate there is no suspended things to exist, thus being effectively filtered to remove caso4.
(2) after in filtrate Deca hydrogen peroxide so that fe in solution2+Sufficiently it is oxidized to fe3+, then Deca ammonia,
Adjust ph value to 5～7, make fe and micro al, mg element is separated out with hydroxide precipitation form and is filtrated to get precipitate.
(3) finally precipitate is used with hydrochloric acidolysiss, the ph value of acid hydrolysis solution controls between 2～4, post-heating make solution
Temperature is increased to 80～100 DEG C, reacts 2～3h, and filtering drying obtains iron-based inhibitor.
Further, in described step (3): salt adding acid adjusts ph value to 3, post-heating make solution temperature be increased to 90
DEG C, react 2h.
Further, application in the coal-fired no discharge of suppression for the iron-based inhibitor of above-mentioned preparation.Specifically: by above-mentioned system
Standby inhibitor, the ratio according to 2-10% is mixed homogeneously with coal, then carries out the burning that final temperature is 900 DEG C in tube furnace
Experiment, and detect the emission performance of nitrogen oxides.
Above-mentioned sulphuric acid, hydrochloric acid and ammonia are analytical reagent, and above-mentioned slag is to collect in each technical process of smelting iron and steel
The vessel slag arriving.
The principles of science of the present invention:
The present invention prepares coal-fired no with vessel slag for primary raw material and discharges the coal-fired method reducing discharging of inhibitor participation, its technology
Key is to be decomposed complex component in vessel slag by the method for acidifying-resolution of precipitate, removes ca first, will wherein have suppression
Component fe, al that no generates etc. is existed in acid hydrolysis solution with ionic formses, as the element source preparing no inhibitor, finally adopts and adds
The method of hydrochloric acid precipitation obtains target product, i.e. the mixture of the iron containing compoundses based on ferrum.The feature of the method is to turn
The multicomponent inhibitor of the main component fe preparation of slag, its chemical composition is mainly fecl3、fecl2、mgcl2Deng, wherein for
fecl3、fecl2Total content is more than 90%, and remaining microcomponent is other doping trace element and acid hemolysis process in vessel slag
The element being mixed into, participates in burning to this inhibitor and plays certain catalytic effect.
Compared with prior art, the present invention has following technical effect that
1st, break through the technology path that tradition is used the chemical reagent and first resource inhibitor as coal-fired suppression no, and with
Metallurgical solid waste-slag is object of study, using key component fe, al in slag and other trace element, using acid
Solution coprecipitation, prepares the additive of suppression coal-fired no discharge, and the raw material breaching traditional additive for fire coal relies on merely
Chemical reagent or the limitation of first resource, while reducing coal-fired no discharge costs, for metallurgical solid waste-vessel slag resource
High value added utilization provides new way.
2nd, use compared with the performance of coal-fired no inhibitor of chemical reagent synthesis or first resource with tradition, institute of the present invention
The fe base fire coal no inhibitor stating new method preparation has preferable suppression emission effect, by small-sized fluidized bed combustion testing,
Emission reduction effect is obvious.
Brief description
Fig. 1 is that the embodiment of the present invention 2 preparation fe base inhibitor participates in coal-fired reduction discharged nitrous oxides figure；
As seen from Figure 1, the amount ratio adding coal with dirt mud based additive increases, and no discharge capacity is decreased obviously, this explanation
The standby inhibitor of prepared from steel slag adds coal-fired process, can effectively suppress the discharge of no, because converter slag addition excessively can be right
Coal sample combustion heat release value has certain reduction, in order that efficiency of combustion and no emission reduction effect reach optimum, therefore, by vessel slag system
Standby fe base fire coal inhibitor adds in coal according to 6% ratio and mixes, and thus demonstrates this nitrogen oxides inhibitor in suppression
Feasibility in coal-fired no draining technology application.
Specific embodiment
Illustrate the present invention below by embodiment, but embodiment is not intended to limit protection scope of the present invention.
Embodiment 1
Take vessel slag below 200 mesh for the 100g granularity, plus sulphuric acid adjusts ph value to 2, stirs 30min, makes in solution
Ca particle is with caso4The form of precipitation separates out, sucking filtration, washing filter cake 2 times, and sucking filtration to filtrate there is no suspended things to exist, thus having
Effect is filtered to remove caso4, afterwards in filtrate Deca hydrogen peroxide so that fe in solution2+Sufficiently it is oxidized to fe3+, then Deca
Ammonia, is adjusted ph value to 5, so that the element such as fe and micro al, mg is separated out with hydroxide precipitation form and be filtrated to get precipitation,
Afterwards precipitate is used with hydrochloric acidolysiss, the ph value of acid hydrolysis solution is 2, post-heating make solution temperature be increased to 80 DEG C, acid hemolysis process
In add the moisture evaporating, keep acidolysis liquid level constant, reaction after 1h terminates, filtering drying obtains the suppression of fe base nitrogen oxides
Agent, pack sealing is standby.
Embodiment 2
Take vessel slag below 200 mesh for the 100g granularity, plus sulphuric acid adjusts ph value to 3, stirs 30min, makes in solution
Ca particle is with caso4The form of precipitation separates out, sucking filtration, washing filter cake 2 times, and sucking filtration to filtrate there is no suspended things to exist, thus having
Effect is filtered to remove caso4, afterwards in filtrate Deca hydrogen peroxide so that fe in solution2+Sufficiently it is oxidized to fe3+, then Deca
Ammonia, is adjusted ph value to 6, so that the element such as fe and micro al, mg is separated out with hydroxide precipitation form and be filtrated to get precipitation,
Afterwards precipitate is used with hydrochloric acidolysiss, the ph value of acid hydrolysis solution is 3, post-heating make solution temperature be increased to 90 DEG C, acid hemolysis process
In add the moisture evaporating, keep acidolysis liquid level constant, reaction after 2h terminates, filtering drying obtains the suppression of fe base nitrogen oxides
Agent, pack sealing is standby.
Embodiment 3
Take vessel slag below 200 mesh for the 100g granularity, plus sulphuric acid adjusts ph value to 4, stirs 30min, makes in solution
Ca particle is with caso4The form of precipitation separates out, sucking filtration, washing filter cake 2 times, and sucking filtration to filtrate there is no suspended things to exist, thus having
Effect is filtered to remove caso4, afterwards in filtrate Deca hydrogen peroxide so that fe in solution2+Sufficiently it is oxidized to fe3+, then Deca
Ammonia, is adjusted ph value to 7, so that the element such as fe and micro al, mg is separated out with hydroxide precipitation form and be filtrated to get precipitation,
Afterwards precipitate is used with hydrochloric acidolysiss, the ph value of acid hydrolysis solution is 4, post-heating make solution temperature be increased to 100 DEG C, acid hemolysis process
In add the moisture evaporating, keep acidolysis liquid level constant, reaction after 3h terminates, filtering drying obtains the suppression of fe base nitrogen oxides
Agent, pack sealing is standby.
Embodiment 4
By the fe base nitrogen oxides inhibitor of preparation and coal mixing 200g, fe base nitrogen oxides inhibitor in embodiment 2
Content accounts for the 2% of mixing coal sample, puts in TG-MS combination instrument, under air atmosphere (flow be 30ml/min) with 10 DEG C/
Min heating rate is heated to 100 DEG C and constant temperature 30min from room temperature, to guarantee that sample is completely dried, then is heated up speed with 10 DEG C/min
Rate is heated to 900 DEG C and constant temperature 20min, to ensure that coal fully burns.
Embodiment 5
By the fe base nitrogen oxides inhibitor of preparation and coal mixing 200g, fe base nitrogen oxides inhibitor in embodiment 2
Content accounts for the 4% of mixing coal sample, puts in TG-MS combination instrument, under air atmosphere (flow be 30ml/min) with 10 DEG C/
Min heating rate is heated to 100 DEG C and constant temperature 30min from room temperature, to guarantee that sample is completely dried, then is heated up speed with 10 DEG C/min
Rate is heated to 900 DEG C and constant temperature 20min, to ensure that coal fully burns.
Embodiment 6
By the fe base nitrogen oxides inhibitor of preparation and coal mixing 200g, fe base nitrogen oxides inhibitor in embodiment 2
Content accounts for the 6% of mixing coal sample, puts in TG-MS combination instrument, under air atmosphere (flow be 30ml/min) with 10 DEG C/
Min heating rate is heated to 100 DEG C and constant temperature 30min from room temperature, to guarantee that sample is completely dried, then is heated up speed with 10 DEG C/min
Rate is heated to 900 DEG C and constant temperature 20min, to ensure that coal fully burns.
Embodiment 7
By the fe base nitrogen oxides inhibitor of preparation and coal mixing 200g, fe base nitrogen oxides inhibitor in embodiment 2
Content accounts for the 8% of mixing coal sample, puts in TG-MS combination instrument, under air atmosphere (flow be 30ml/min) with 10 DEG C/
Min heating rate is heated to 100 DEG C and constant temperature 30min from room temperature, to guarantee that sample is completely dried, then is heated up speed with 10 DEG C/min
Rate is heated to 900 DEG C and constant temperature 20min, to ensure that coal fully burns.
Embodiment 8
By the fe base nitrogen oxides inhibitor of preparation and coal mixing 200g, fe base nitrogen oxides inhibitor in embodiment 2
Content accounts for the 10% of mixing coal sample, puts in TG-MS combination instrument, with 10 under air atmosphere (flow is 30ml/min)
DEG C/min heating rate is heated to 100 DEG C and constant temperature 30min from room temperature, to guarantee that sample is completely dried, then with 10 DEG C/min liter
Warm speed is heated to 900 DEG C and constant temperature 20min, to ensure that coal fully burns.
Claims (3)
1. a kind of method preparing iron-based inhibitor for primary raw material with metallurgical converter slag extract, the method concrete steps are such as
Under:
(1) first ball milling is carried out to metallurgical converter slag, make sample granularity reach below 200 mesh, then this slag is added sulphuric acid
Adjust ph value to 2～4, stir 30min, make the ca particle in solution with caso4The form of precipitation separates out, sucking filtration, washs filter cake 2
Secondary, sucking filtration to filtrate there is no suspended things to exist, thus being effectively filtered to remove caso4；
(2) after in filtrate Deca hydrogen peroxide so that fe in solution2+Sufficiently it is oxidized to fe3+, then Deca ammonia, adjust
Ph value, to 5～7, makes fe and micro al, and mg element is separated out with hydroxide precipitation form and is filtrated to get precipitate；
(3) finally precipitate is used with hydrochloric acidolysiss, the ph value of acid hydrolysis solution controls between 2～4, post-heating make solution temperature
It is increased to 80～100 DEG C, reacts 2～3h, filtering drying obtains iron-based inhibitor.
2. the method as claimed in claim 1 iron-based inhibitor being prepared for primary raw material with metallurgical converter slag extract, its
Be characterised by, in described step (3): salt adding acid adjusts ph value to 3, post-heating make solution temperature be increased to 90 DEG C, react 2h.
3. the iron-based inhibitor prepared for primary raw material with metallurgical converter slag extract as claimed in claim 1 is in suppression combustion
Application in coal no discharge.
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| CN101440321A (en) * | 2008-12-18 | 2009-05-27 | 东华大学 | Efficient reburning denitration mixed fuel made from scrap tire and preparation thereof |
| CN102240505A (en) * | 2011-07-13 | 2011-11-16 | 东华大学 | Method for reducing NO by using iron catalyst |
| CN104826481A (en) * | 2015-05-13 | 2015-08-12 | 中国科学院过程工程研究所 | Combined desulfurization and denitrification method implemented by using metallurgical slags |
| CN104946339A (en) * | 2015-05-27 | 2015-09-30 | 上海理工大学 | Method for controlling biomass combustion NO by using nano iron-base additive |
| CN105327926A (en) * | 2015-10-27 | 2016-02-17 | 安徽工业大学 | Method for preparing calcium-ferrum double-oxygen carrier with converter steelmaking slag as raw materials |
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2016
- 2016-10-08 CN CN201610877363.2A patent/CN106367154B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060228282A1 (en) * | 2005-04-12 | 2006-10-12 | Bing Zhou | Method for reducing NOx during combustion of coal in a burner |
| CN101161331A (en) * | 2006-10-10 | 2008-04-16 | 辽宁科技大学 | Method for processing low concentration unwanted waste gas using microwave-solid castoff |
| CN101440321A (en) * | 2008-12-18 | 2009-05-27 | 东华大学 | Efficient reburning denitration mixed fuel made from scrap tire and preparation thereof |
| CN102240505A (en) * | 2011-07-13 | 2011-11-16 | 东华大学 | Method for reducing NO by using iron catalyst |
| CN104826481A (en) * | 2015-05-13 | 2015-08-12 | 中国科学院过程工程研究所 | Combined desulfurization and denitrification method implemented by using metallurgical slags |
| CN104946339A (en) * | 2015-05-27 | 2015-09-30 | 上海理工大学 | Method for controlling biomass combustion NO by using nano iron-base additive |
| CN105327926A (en) * | 2015-10-27 | 2016-02-17 | 安徽工业大学 | Method for preparing calcium-ferrum double-oxygen carrier with converter steelmaking slag as raw materials |
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