CN107913680A - A kind of preparation method of flue gas dearsenification adsorbent - Google Patents

A kind of preparation method of flue gas dearsenification adsorbent Download PDF

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Publication number
CN107913680A
CN107913680A CN201711220671.9A CN201711220671A CN107913680A CN 107913680 A CN107913680 A CN 107913680A CN 201711220671 A CN201711220671 A CN 201711220671A CN 107913680 A CN107913680 A CN 107913680A
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adsorbent
flue gas
prepared
flyash
mixing
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CN107913680B (en
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凌海涛
王海军
彭世恒
常立忠
徐蕊
周俐
王建军
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YANGZHOU XINXIN METALLURGICAL EQUIPMENT MANUFACTURING CO.,LTD.
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Anhui University of Technology AHUT
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42Materials comprising a mixture of inorganic materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes

Abstract

A kind of preparation method of flue gas dearsenification adsorbent of the present invention, flue gas dearsenic technique field.Step 1 raw material mixing of the present invention mixes:Adsorbent is prepared in calcium oxide, metallurgical slag, zeolite and flyash after mixing and mixes material;Step 2 is pelletized:The adsorbent being prepared in step 1 is mixed material to add in cylindrical mixer, absorbent particles are prepared after the completion of mixing granulation;Step 3 pre-processes:The absorbent particles being prepared in step 2 are heated to 800 900 DEG C, adsorbent are obtained after the completion of cooling, the addition of flyash is M4=γ (M1+ α M2 δ M3) β/(1 α) M2.The invention enables arsenic and its oxide to provide the longer reaction time in the extended residence time on the surface of adsorbent, the reaction for adsorbent and arsenic and its oxide, promote the reaction process of calcium oxide and arsenic, improve adsorption effect of the adsorbent to arsenic.

Description

A kind of preparation method of flue gas dearsenification adsorbent
Technical field
The invention belongs to smoke pollution removing sulfuldioxide field, relate in particular to, a kind of preparation of flue gas dearsenification adsorbent Method.
Background technology
A large amount of SO in flue gas2, NOxDeng pollutant, since discharge capacity is huge, concentration is high, people very early carry out it Relatively research work and achieve significant achievement.As environmental protection pressure is increasing, researcher has found to be enriched in flue gas Trace element enter air after, can equally cause great bodily injury to human body and environment, be primarily due to trace element have it is heavy Shallow lake property, migrating property, are easily enriched to the other particle surface of micron, submicron order, formed in an atmosphere colloidal sol and long-term suspension its In, cause serious respiratory disease into human lung.
Wherein, arsenic is the global contaminant of great harm, has extremely strong bioaccumulation and carcinogenic teratogenesis, is prestige Coerce human health and the great environmental problem of ecological safety.Micro arsenic oxide will make one poisoning (regulation air in air Middle arsenic content is no more than 0.003mg/L), it is damaged nervous system, severe one is even dead.The 60% of total arsenic load in air~ 75% is as caused by human activity factor.Wherein, metal smelt occupies the overwhelming majority, about 35%~65%.Therefore it is badly in need of opening The research of flue gas dearsenification is opened up, explores rational arsenic pollution control measure.
Through retrieval, there is similar scheme to disclose;Such as:Arsenic, the device of mercury and dearsenification, the method for mercury in a kind of removing flue gas (application number:201310750980.2 the applying date:2013.12.31), it includes denitrating system, deduster, magnetic separator, machine Tool screening machine and spraying system, denitrating system are connected with burner hearth, and the outlet of denitrating system is connected with the entrance of deduster, deduster It is connected with magnetic separator, mechanical sieving machine, before magnetic separator, mechanical sieving machine are by spraying system and denitrating system entrance Pipeline be connected.It can not only effectively remove the gaseous state arsenic in flue gas, while the Elemental Mercury in energy catalysis oxidation flue gas.The skill Although art can two kinds of pollutants of emission reduction arsenic and mercury, not special dearsenification at the same time adsorbent, cause the emission reduction of arsenic to imitate Fruit needs to be further improved.
A kind of in addition, industrial smoke dust-removal and desulfurizing dearsenification integral method (application number:201410557222.3 the applying date: 2014.10.20), it absorbs SOx using inorganic sulphide, while the grit in flue gas is trapped, the same cigarette of inorganic sulphide The reaction of the toxic heavy metals such as mercury, arsenic in gas is raw insoluble into sulphurizing salt, then using being complexed ferrous absorption NOx, inorganic sulphide Thing is as reducing agent absorbent regeneration.Be conducive to the removing of the Toxics such as dust, SOx, NOx, mercury, arsenic.Although the technology can be with Emission reduction multiple pollutant at the same time, but the adsorbent of unspecial dearsenification, cause the emission reduction effect of arsenic to need further to be carried It is high.
The content of the invention
1. technical problems to be solved by the inivention
It is an object of the present invention to overcome in the prior art without the adsorbent of special flue gas dearsenification, cause flue gas The problem of dearsenification effect is limited, there is provided a kind of preparation method of flue gas dearsenification adsorbent, by calcium oxide, metallurgical slag, zeolite and Flyash is prepared adsorbent and mixes material after mixing, then adsorbent is mixed in material addition cylindrical mixer and is prepared Absorbent particles, pass through the cooperation of calcium oxide, metallurgical slag, zeolite and flyash so that adsorbent passes through chemisorbed and thing Reason absorption is combined, and greatly improves the adsorption effect of adsorbent.
2. technical solution
To reach above-mentioned purpose, technical solution provided by the invention is:
A kind of preparation method of flue gas dearsenification adsorbent of the present invention, calcium oxide, metallurgical slag, zeolite and flyash are mixed Adsorbent is prepared after closing uniformly and mixes material, then adsorbent mixing material is added in cylindrical mixer adsorbent is prepared Grain.
Preferably, specific preparation method is:
Step 1:Raw material mixing mixes
Adsorbent is prepared in calcium oxide, metallurgical slag, zeolite and flyash after mixing and mixes material;
Step 2:Granulation
The adsorbent being prepared in step 1 is mixed material to add in cylindrical mixer, and water is added in batch mixer, Absorbent particles are prepared after the completion of mixing granulation;
Step 3:Pretreatment
The absorbent particles being prepared in step 2 are heated to 800-900 DEG C, adsorbent is obtained after the completion of cooling.
Preferably, step 1:What raw material mixing mixed concretely comprises the following steps:
(1) mixture A is prepared:Calcium oxide, metallurgical slag and zeolite are weighed by mass fraction to be added sequentially in mixer, Mixture A is uniformly made afterwards in stirrer for mixing;
(2) flyash pre-processes:Flyash is added in sodium hydroxide solution, the concentration of sodium hydroxide solution is 1.5mol/L, modified coal ash is obtained after dry;
(3) flyash is added into mixture A, then additive is added in above-mentioned mixture again, mixing is equal Adsorbent is prepared after even and mixes material.
Preferably, step 3:Pretreatment concretely comprises the following steps:The absorbent particles being prepared in step 2 are placed into In micro-wave oven, and microwave heating is carried out under conditions of nitrogen protection, be heated to 800-900 DEG C, keep the temperature 30min, cooling is completed After obtain adsorbent.
Preferably, the addition of flyash is M4=γ (M1+ α M2- δ M3)-β/(1- α) M2, wherein:M1 is calcium oxide Quality, M2 are the quality of metallurgical slag, and M3 is the quality of zeolite;It is in metallurgical slag that γ, which takes 0.15~0.25, δ to take 1.5-2, α, CaO and MgO mass percentages;β is the Fe in metallurgical slag2O3With MnO mass percentages.
Preferably, the mass ratio of calcium oxide and metallurgical slag is 2.2~4.0.
Preferably, additive is further included, the additive includes blast furnace ash, chromium slag and mullite.
Preferably, the addition of the additive is the 2-5% of adsorbent.
Preferably, accelerating agent is further included, the accelerating agent is more than 1000 organic matter for draw ratio..
3. beneficial effect
Using technical solution provided by the invention, compared with prior art, have the advantages that:
(1) a kind of preparation method of flue gas dearsenification adsorbent of the invention, adsorbent allow arsenic and its oxide to exist The extended residence time on the surface of adsorbent, the reaction for adsorbent and arsenic and its oxide provide the longer reaction time, The alkali metal in flyash can promote the electronic migration of calcium oxide under the high temperature conditions, and the room for promoting arsenic atom to enter O Either bridge location or the top position into Ca, promote the reaction process of calcium oxide and arsenic, form Ca-As compounds:Ca (AsO2)2、Ca3(AsO4)2、Ca2As2O7And Ca3As2O8;At the same time, flyash and vessel slag collective effect, promote iron oxygen The decomposition of compound, and a large amount of metal promoteds in flyash vessel slag surface forms substantial amounts of reaction contact position, promotes Arsenic and its oxide are reacted with ferriferous oxide or the calcium oxide of vessel slag activity, improve adsorption effect of the adsorbent to arsenic;
(2) preparation method of a kind of flue gas dearsenification adsorbent of the invention, a large amount of active ingredients in vessel slag not only may be used It to promote the combination of arsenic and its oxide and calcium oxide and vessel slag, and can directly be reacted, and then be improved with arsenic The adsorption effect of chemisorbed;Arsenic and its oxide is fixed in chemisorbed so that and the arsenic content of adsorbent surface reduces, And then the progress of physical absorption is promoted, improve adsorption effect of the adsorbent to arsenic.
Brief description of the drawings
Fig. 1 is a kind of structure chart of adsorption tower for flue gas dearsenification of the present invention;
Fig. 2 is a kind of preparation flow figure of adsorbent for flue gas dearsenification of the present invention.
Label declaration in schematic diagram:
110th, air inlet;111st, except water layer;120th, equal fluid layer;121st, venthole;122nd, transverse slat;123rd, side plate;130th, it is steady Fluid layer;140th, activated carbon adsorption layer;150th, the adsorbent bed of material;160th, gas outlet;
210th, electro-resistive heating element;220th, microwave heating element;230th, gap is heated.
Embodiment
Attached drawing hereafter with reference to the detailed description of the exemplary embodiment of the present invention, which forms one of description Point, in the figure the enforceable exemplary embodiment of the present invention is shown as example.Although these exemplary embodiment quilts Fully describe in detail so that those skilled in the art can implement the present invention, it is to be understood that can realize other embodiment and Can without departing from the spirit and scope of the present invention to the present invention various changes can be made.Hereafter to the embodiment of the present invention More detailed description is not limited to required the scope of the present invention, and just to be illustrated and do not limit pair The description of the features of the present invention and feature, to propose to perform the best mode of the present invention, and is sufficient so that those skilled in the art It can implement the present invention.Therefore, the scope of the invention is only defined by the appended claims.
Hereafter detailed description of the present invention and example embodiment can be more fully understood with reference to attached drawing, wherein the present invention Element and feature are identified by reference numeral.
Embodiment 1
A kind of adsorbent for flue gas dearsenification of the present invention, including calcium oxide, metallurgical slag, zeolite and flyash.Powder The addition of coal ash is M4=γ (M1+ α M2- δ M3)-β/(1- α) M2, wherein:M1 is the quality of calcium oxide, and M2 is metallurgical slag Quality, M3 be zeolite quality;γ takes 0.15~0.25, δ to take 1.5-2, wherein it is worth noting that:α is in metallurgical slag CaO and MgO mass percentages;β is the Fe in metallurgical slag2O3With MnO mass percentages.The matter of calcium oxide and zeolite The ratio between amount is 4~8, and the present embodiment takes 5.
The calcium oxide 60kg of the present embodiment, metallurgical slag 20kg, zeolite 12kg;The quality that flyash is calculated is:M4 =γ (60+ α 20- δ 12)-β/(1- α) 20=8.14kg wherein γ take 0.2, δ to take 1.5, and flyash has larger ratio surface Product, flyash and zeolite have preferable suction-operated to arsenic so that arsenic and its oxide can be in the stops on the surface of adsorbent Time lengthening, the reaction for adsorbent and arsenic and its oxide provide the longer reaction time.And flyash and calcium oxide Collective effect, the alkali metal in flyash can promote the electronic migration of calcium oxide under the high temperature conditions, and promote arsenic atom Either bridge location or enter the top position of Ca into the room of O, promote the reaction process of calcium oxide and arsenic, it is compound to form Ca-As Thing:Ca(AsO2)2、Ca3(AsO4)2、Ca2As2O7And Ca3As2O8, which can occur under certain conditions Mutually convert.At the same time, flyash and vessel slag collective effect, promote the decomposition of ferriferous oxide, and big in flyash Amount metal promoted vessel slag surface forms substantial amounts of reaction contact position, promote arsenic and its oxide and ferriferous oxide or The calcium oxide reaction of vessel slag activity;In addition, a large amount of active ingredients in vessel slag can not only promote arsenic and its oxide with The combination of calcium oxide and vessel slag, and can directly be reacted with arsenic, and then improve the adsorption effect of chemisorbed;Change Learn absorption arsenic and its oxide is fixed so that the arsenic content of adsorbent surface reduces, and then promotes physical absorption Carry out, both complement each other, so as to improve adsorption effect, and then improve adsorption effect of the adsorbent to arsenic, and may send out Raw following reaction:
4AsO(g)+O2(g)+2CaO=2Ca (AsO2)2
4/3A8O(g)+O2(g)+2CaO=2/3Ca3(AsO4)2
3AsO(g)+2.5O2(g)+2Fe3O4=3FeAsO4
4/3AsO(g)+O2(g)+2MgO=2/3Mg3(AsO4)2
4AsO(g)+O2(g)+2MgO=2Mg (AsO2)2
As2O3(g)+3CaO+O2(g)=Ca3(AsO4)2
2CaO+1/2As4O4(g)+O2=Ca2As2O7(s)
But on the other hand, since the addition of flyash will block greatly very much the absorption duct of adsorbent so that absorption Effect is deteriorated, and have impact on transmittance process of the physical absorption to chemisorbed, therefore, during this controls the composition in adsorbent It is particularly important that, thus the present invention by long-term research and design M4=γ (M1+ α M2- δ M3)-β/(1- α) M2, and to each Component is regulated and controled;The metallurgical slag is vessel slag, and the percentage composition of vessel slag is CaO:43.5%, SiO2:15.5%; Al2O3:3.8%;MgO:3.4%;Fe2O3:5.2%;MnO:2.4%;Remaining is impurity.
Metallurgical slag is vessel slag, the Fe in vessel slag2O3Mass percentage be more than 5%.Granularity is 0.074- The percentage composition of the vessel slag of 5.0mm is more than 50%.Vessel slag granularity is formed by following mass percentage:Granularity≤ 0.074mm:5%, 0.074-3.0mm:25%, 3.0-5.0mm:40%;5.0-10.0mm:30%.
The flyash of the present embodiment is before coal-fired flue-gas is discharged into air by air-introduced machine, and chilling is thin in vitreum state Grain, by deduster, is separated, collects obtained particulate, the mass percentage of the fine coal ash component is:SiO2:45.2%, Al2O3:28.6%, Fe2O3:8.7%, CaO:7.4%, MgO:3.6%, Na2O+K2O:2.5%, remaining is impurity.The powder Coal ash using sodium hydroxide either potassium hydroxide be modified processing modifying agent be sodium hydroxide or potassium hydroxide;This implementation The processing method of flyash of example is:Flyash is added in sodium hydroxide solution, (high pressure is under elevated pressure conditions 150~200KPa), 120 DEG C of reaction 0.5-1h are heated to, dry 2h after the completion of reaction under conditions of 105 DEG C, obtain modified powder Coal ash.
Metallurgical slag is vessel slag, the Fe in vessel slag2O3Mass percentage be more than 5%.Granularity is 0.074- The percentage composition of the vessel slag of 5.0mm is more than 50%.Vessel slag granularity is formed by following mass percentage:Granularity≤ 0.074mm:5%, 0.074-3.0mm:25%, 3.0-5.0mm:40%;5.0-10.0mm:30%.
The flyash of the present embodiment is before coal-fired flue-gas is discharged into air by air-introduced machine, and chilling is thin in vitreum state Grain, by deduster, is separated, collects obtained particulate, the mass percentage of the fine coal ash component is:SiO2:45.2%, Al2O3:28.6%, Fe2O3:8.7%, CaO:7.4%, MgO:3.6%, Na2O+K2O:2.5%, remaining is impurity.The powder Coal ash using sodium hydroxide either potassium hydroxide be modified processing modifying agent be sodium hydroxide or potassium hydroxide;This implementation The processing method of flyash of example is:Flyash is added in sodium hydroxide solution, (high pressure is under elevated pressure conditions 150~200KPa), 120 DEG C of reaction 0.5-1h are heated to, dry 2h after the completion of reaction under conditions of 105 DEG C, obtain modified powder Coal ash.
As shown in Fig. 2, the preparation method of the adsorbent of the present embodiment is:
Step 1:Raw material mixing mixes
(1) mixture A is prepared:Calcium oxide, metallurgical slag and zeolite are weighed by mass fraction to be added sequentially in mixer, Mixture A is uniformly made afterwards in stirrer for mixing;
(2) flyash pre-processes:Flyash is added in sodium hydroxide solution, the concentration of sodium hydroxide solution is 1.5mol/L, 120 DEG C of reaction 0.5-1h are heated under the conditions of 150~200KPa, are done after the completion of reaction under conditions of 105 DEG C Dry 2h, obtains modified coal ash;
(3) quality of flyash is calculated according to formula:M4=γ (M1+ α M2- δ M3)-β/(1- α) M2, wherein:M1 is oxygen Change the quality of calcium, M2 is the quality of metallurgical slag, and M3 is the quality of zeolite;It is metallurgical that γ, which takes 0.15~0.25, δ to take 1.5-2, α, CaO and MgO mass percentages in clinker;β is the Fe in metallurgical slag2O3With MnO mass percentages;By flyash plus Enter into mixture A, adsorbent is prepared after mixing and mixes material;
Step 2:Granulation
The adsorbent being prepared in step 1 is mixed material to add in cylindrical mixer, and water is added in batch mixer, Absorbent particles are prepared after the completion of mixing granulation;
Step 3:Pretreatment
The absorbent particles being prepared in step 2 are placed into micro-wave oven, and are carried out under conditions of nitrogen protection Microwave heats, and is heated to 800 DEG C, keeps the temperature 30min;Its specific heating steps is as follows:
First, with the programming rate of 5 DEG C/min, 250 DEG C are warming up to, keeps the temperature 10min;
Secondly, with the programming rate of 10 DEG C/min, 800 DEG C are warming up to, keeps the temperature 30min;Adsorbent is obtained after the completion of cooling; The adsorbent being prepared by above-mentioned method so that adsorbent surface Ca-O, Si-O, Fe-O and Al-O are in high energy shape State, so as to improve the absorption property of adsorbent.Flue gas passes through adsorbent, the present embodiment selection under conditions of 400~900 DEG C Temperature be 800 DEG C, the thickness of feed layer of adsorbent is 500mm, flue gas flow 0.2L/min;The content of arsenic in entrance flue gas For 3mg/L;The content of arsenic is 0.58mg/L in the flue gas of exit, and emission reduction efficiency reaches 80.67%.
Embodiment 2
The same embodiment of substance of the present embodiment, difference are:Additive is further included, the additive includes Blast furnace ash, chromium slag and mullite;Each component is formed according to following mass parts:Blast furnace ash:60%th, chromium slag:20%th, mullite: 20%.Additive is added by the way of matching somebody with somebody outside, and the addition of additive is the 1-2% of adsorbent, the present embodiment 1%, i.e., The addition of additive is the 1-2% of the sum of calcium oxide, metallurgical slag, zeolite and flyash quality.Under high temperature bar, additive In the electronics that promotes under the high temperature conditions in flyash and vessel slag of metallic element shift, so as to promote in flue gas Arsenic element enter calcium oxide in O room and bridge location, adsorption effect of the adsorbent to arsenic is improved, in addition in additive Metal promoted flying dust in arsenic enter in vitreous aluminosilicate mineral lattice, with AsO4 -3Form be present in adsorbent In;And the Mullite Powder in additive can be attached to the surface of vessel slag or calcium oxide, vessel slag, calcium oxide with Promote under the collective effect of mullite in mullite lattice;In addition, there are substantial amounts of alkali metal in blast furnace ash and chromium slag, NaAs can be formed with arsenic3O8, KAs3O8, K3AsO4Etc. compound, with reaction generation therein moieties performance simultaneously Be not very stable, but the of short duration adsorption effect of adsorbent exactly improved using these intermediate products so that arsenic and its Oxide can be adsorbed in the surface of adsorbent, and add the residence time of arsenic and its oxide in adsorbent surface, and be The chemisorbed of adsorbent provides the foundation.Flue gas under conditions of 400~900 DEG C by adsorbent, the present embodiment selection Temperature is 400 DEG C, and the thickness of feed layer of adsorbent is 500mm, flue gas flow 0.2L/min;The content of arsenic is in entrance flue gas 2mg/L;The content of arsenic is 0.35mg/L in the flue gas of exit, and emission reduction efficiency reaches 82.50%.
The specific preparation method of the adsorbent of the present invention is as follows:
Step 1:Raw material mixing mixes
(1) mixture A is prepared:Calcium oxide, metallurgical slag and zeolite are weighed by mass fraction to be added sequentially in mixer, Mixture A is uniformly made afterwards in stirrer for mixing;
(2) flyash pre-processes:Flyash is added in sodium hydroxide solution, the concentration of sodium hydroxide solution is 1.5mol/L, 120 DEG C of reaction 0.5-1h are heated under the conditions of 150~200KPa, are done after the completion of reaction under conditions of 105 DEG C Dry 2h, obtains modified coal ash;
(3) blast furnace ash, chromium slag and mullite is weighed by mass fraction to be uniformly mixed, and in sodium hydroxide solution into Row cleaning, is dried to obtain additive after the completion of cleaning;
(4) quality of flyash is calculated according to formula:M4=γ (M1+ α M2- δ M3)-β/(1- α) M2, wherein:M1 is oxygen Change the quality of calcium, M2 is the quality of metallurgical slag, and M3 is the quality of zeolite;It is metallurgical that γ, which takes 0.15~0.25, δ to take 1.5-2, α, CaO and MgO mass percentages in clinker;β is the Fe in metallurgical slag2O3With MnO mass percentages;By flyash plus Enter into mixture A, then additive is added in above-mentioned mixture again, adsorbent mixing is prepared after mixing Material;
Step 2:Granulation
The adsorbent being prepared in step 1 is mixed material to add in cylindrical mixer, and water is added in batch mixer, Absorbent particles are prepared after the completion of mixing granulation;
Step 3:Pretreatment
The absorbent particles being prepared in step 2 are placed into micro-wave oven, and are carried out under conditions of nitrogen protection Microwave heats, and is heated to 800-900 DEG C, and the present embodiment selects 900 DEG C, keeps the temperature 30min;Its specific heating steps is as follows:
First, with the programming rate of 5 DEG C/min, 300 DEG C are warming up to, keeps the temperature 10min;
Secondly, with the programming rate of 10 DEG C/min, 900 DEG C are warming up to, keeps the temperature 30min;Adsorbent is obtained after the completion of cooling.
Embodiment 3
The substance of the present embodiment further includes accelerating agent, the accelerating agent is more than 1000 for draw ratio with embodiment 1 Organic matter.For plant fiber, either animal hair fiber or plastic optical fibre, accelerating agent use outer the accelerating agent of the present embodiment The mode matched somebody with somebody adds, and the addition of accelerating agent is the 0.05-0.2% of adsorbent, and the present embodiment 0.1%, i.e. accelerating agent add Enter 0.05-0.2% of the amount for the sum of calcium oxide, metallurgical slag, zeolite and flyash quality;The present embodiment use for animal wool The mass ratio of the mixture of hair fiber and cotton fiber, hair fiber and cotton fiber is 2:1;By adding hair in adsorbent Fiber and cotton fiber, can make it that distribution is larger mesoporous in the absorption after processing, substantially increases the ratio of the absorption of adsorbent Surface area, can improve the adsorption effect of adsorbent;In addition so that be interconnected between duct, so as to promote physical absorption Conversion to chemisorbed, not only increases the effect of chemisorbed, and promotes the lasting progress of physical absorption;And then carry The high adsorption effect of adsorbent.Flue gas under conditions of 400~900 DEG C by adsorbent, the temperature of the present embodiment selection for 700 DEG C, the thickness of feed layer of adsorbent is 500mm, flue gas flow 0.2L/min;The content of arsenic is 4mg/L in entrance flue gas; The content of arsenic is 0.45mg/L in the flue gas of exit, and emission reduction efficiency reaches 88.75%.
Embodiment 4
The same embodiment of substance of the present embodiment, difference are:Additive include blast furnace ash, chromium slag, mullite, The mass percentage of sepiolite, carbonitride, wherein each component is:Blast furnace ash:50%, chromium slag:20%;Mullite:10%, sea Afrodite:10%;Carbonitride:10%, additive is added by the way of matching somebody with somebody outside, and the addition of additive is the 1.5% of adsorbent. Additive can improve the specific surface area in adsorbent physical adsorption process, so as to improve the adsorption effect of adsorbent;Flue gas By adsorbent under conditions of 400~900 DEG C, the temperature of the present embodiment selection is 600 DEG C, and the thickness of feed layer of adsorbent is 500mm, flue gas flow 0.2L/min;The content of arsenic is 2mg/L in entrance flue gas;The content of arsenic is in the flue gas of exit 0.308mg/L, emission reduction efficiency reach 84.60%.
Embodiment 5
The same embodiment of substance of the present embodiment, difference are:Additive include blast furnace ash, chromium slag, mullite, The mass percentage of sepiolite, iron scale, wherein each component is:Blast furnace ash:50%, chromium slag:20%;Mullite:10%, Sepiolite:5%;Iron scale:15%, additive is added by the way of matching somebody with somebody outside, and the addition of additive is adsorbent 1.8%.Additive can improve the specific surface area in adsorbent physical adsorption process, so as to improve the absorption effect of adsorbent Fruit, iron scale improve the chemical reaction process of absorption, improve adsorption effect;Flue gas passes through under conditions of 400~900 DEG C Adsorbent, the temperature of the present embodiment selection is 700 DEG C, and the thickness of feed layer of adsorbent is 600mm, flue gas flow 0.2L/min; The content of arsenic is 2mg/L in entrance flue gas;The content of arsenic is 0.29mg/L in the flue gas of exit, and emission reduction efficiency reaches 85.50%.
Embodiment 6
The same embodiment of substance of the present embodiment, difference are:Additive include blast furnace ash, chromium slag, mullite, The mass percentage of sepiolite, attapulgite, wherein each component is:Blast furnace ash:50%, chromium slag:20%;Mullite:10%, Iron scale:10%;Attapulgite:10%, additive is added by the way of matching somebody with somebody outside, and the addition of additive is adsorbent 2%.Attapulgite has the clay mineral of zeopan containing Shuifu County of chain layer structure, by a series of heating, addition Agent can improve the specific surface area in adsorbent physical adsorption process, so as to improve the adsorption effect of adsorbent, iron scale The chemical reaction process of absorption is improved, improves adsorption effect;Flue gas passes through adsorbent, this reality under conditions of 400~900 DEG C The temperature for applying example selection is 600 DEG C, and the thickness of feed layer of adsorbent is 500mm, flue gas flow 0.2L/min;In entrance flue gas The content of arsenic is 3mg/L;The content of arsenic is 0.47mg/L in the flue gas of exit, and emission reduction efficiency reaches 84.33%.
Embodiment 7
The same embodiment of substance of the present embodiment, difference are:Sinter return fine is further included in adsorbent, sintering returns The addition of ore deposit is the 5-10% of calcium oxide, and the present embodiment 5%, the sinter return fine is that the sintering that granularity is 3-5mm returns Ore deposit, and by sinter return fine smalls to 1-3mm;The raw material mixing mixing method of the present embodiment is:
(1) mixture A is prepared:Calcium oxide, metallurgical slag and zeolite are weighed by mass fraction to be added sequentially in mixer, Mixture A is uniformly made afterwards in stirrer for mixing;
(2) flyash pre-processes:Flyash is added in sodium hydroxide solution, the concentration of sodium hydroxide solution is 1.5mol/L, 120 DEG C of reaction 0.5-1h are heated under the conditions of 150~200KPa, are done after the completion of reaction under conditions of 105 DEG C Dry 2h, obtains modified coal ash;
(3) quality of flyash is calculated according to formula:M4=γ (M1+ α M2- δ M3)-β/(1- α) M2, wherein:M1 is oxygen Change the quality of calcium, M2 is the quality of metallurgical slag, and M3 is the quality of zeolite;It is metallurgical that γ, which takes 0.15~0.25, δ to take 1.5-2, α, CaO and MgO mass percentages in clinker;β is the Fe in metallurgical slag2O3With MnO mass percentages;By flyash with Sinter return fine is mixed, and the mixture of flyash and sinter return fine is added into mixture A, is prepared into after mixing Mix and expect to adsorbent.Sinter return fine provides substantial amounts of reaction duct for adsorbent, improves the adsorption surface area of adsorbent, So as to improve the adsorption effect of adsorbent;Flue gas under conditions of 400~900 DEG C by adsorbent, the present embodiment selection Temperature is 500 DEG C, and the thickness of feed layer of adsorbent is 600mm, flue gas flow 0.2L/min;The content of arsenic is in entrance flue gas 4mg/L;The content of arsenic is 0.72mg/L in the flue gas of exit, and emission reduction efficiency reaches 81.75%.
Embodiment 8
A kind of adsorption tower for flue gas dearsenification of the present embodiment, the bottom of towe of adsorption tower are provided with air inlet 110, and tower top is set There is gas outlet 160;Adsorption tower tower body is disposed with current stabilization layer 130, activated carbon adsorption layer 140, the adsorbent bed of material from the bottom to top 150;I.e. the adsorbent bed of material 150 is arranged at the side away from air inlet 110, and activated carbon adsorption layer 140 is than the adsorbent bed of material 150 more Close to air inlet 110, the flue gas being cleaned is entered in adsorption tower by air inlet 110, and flue gas first passes through current stabilization layer 130 and carries out surely Stream, then adsorption treatment is carried out by activated carbon adsorption layer 140, finally adsorbed again in the adsorbent bed of material 150, so as to improve The adsorption effect of adsorption tower.
Current stabilization layer 130 is used to stablize flue gas stream so that the uniform branch of gas is in adsorption tower so that activated carbon adsorption Layer 140 and the adsorbent bed of material 150 can uniformly be reacted with flue gas, and dress is covered with activated carbon in activated carbon adsorption layer 140 Grain;The dress of the adsorbent bed of material 150 is covered with adsorbent, and the adsorbent is the above-mentioned adsorbent for flue gas dearsenification;Adsorption tower Top on the outside of tower body is provided with microwave heating element 220, and the lower part on the outside of adsorption tower tower body is provided with electro-resistive heating element 210;Wherein microwave heating element 220 and the top of the adsorbent bed of material 150 is correspondingly arranged, i.e. the outside circle of the adsorbent bed of material 150 It is provided with microwave heating element 220 week;The heating-up temperature of microwave heating element 220 is 400~900 DEG C.
Electro-resistive heating element 210 is correspondingly arranged with the lower part of the adsorbent bed of material 150 and activated carbon adsorption layer 140.Adsorb The lower part of the agent bed of material 150 and the outer circumference of activated carbon adsorption layer 140 are provided with electro-resistive heating element 210, electro-resistive heating element 210 heating-up temperature is 120~160 DEG C;It is worth noting that electro-resistive heating element 210 is across activated carbon adsorption layer 140 and prolongs Extend the bottom of the adsorbent bed of material 150;And it is empty that heating is provided between microwave heating element 220 and electro-resistive heating element 210 Gap 230, heating gap 230 can cause there is interval and transition between microwave heating element 220 and electro-resistive heating element 210, So that fluctuation of the flue gas by generation temperature during activated carbon adsorption layer 140 to the adsorbent bed of material 150, so as to promote air flow direction Fluctuation, lays the first stone to improve dearsenification effect.Further it should be noted that it is additionally provided between current stabilization layer 130 and air inlet 110 Equal fluid layer 120, is provided with except water layer 111 on air inlet 110, except water layer 111 is used to remove the moisture in flue gas;The equal fluid layer 120 include transverse slat 122 and side plate 123;Angle between transverse slat 122 and side plate 123 is 120 ° -150 °, transverse slat 122 and side plate 123 surround trapezoidal equal fluid layer 120, and venthole 121 is uniformly provided with equal fluid layer 120;Flue gas is entered by air inlet 110 to be inhaled Enter in attached tower and then by equal fluid layer 120 in adsorption tower tower body, flue gas passes through current stabilization layer 130, in 150 cigarette of the adsorbent bed of material Arsenic and its oxide in gas are adsorbed by adsorbent;The heating-up temperature of the microwave heating element 220 of the present embodiment is 700 DEG C; The bottom of the adsorbent bed of material 150 and the outer circumference of activated carbon adsorption layer 140 are provided with electro-resistive heating element 210, resistance heating The heating-up temperature of component 210 is 140 DEG C.Used adsorbent is the adsorbent in embodiment 1, and arsenic contains in entrance flue gas Measure as 4mg/L;The content of arsenic is 0.74mg/L in the flue gas of exit, and emission reduction efficiency reaches 81.50%.Inhaled using the heating of multistage It is attached, and be combined using adsorbent and physical absorption, improve the adsorption effect of adsorbent.
The present invention is described in detail above in conjunction with specific exemplary embodiment.It is understood, however, that it can not take off Various modifications and variations are carried out in the case of from the scope of the present invention being defined by the following claims.Detailed description and drawings Should be to be considered only as it is illustrative and not restrictive, if there is any such modifications and variations, then they all will Fall into the scope of the present invention described here.In addition, background technology is intended to Development Status and meaning in order to illustrate this technology, It is not intended to limit the application field of the present invention or the application and the present invention.
More specifically, although the exemplary embodiment of the present invention has been described herein, but the invention is not limited in These embodiments, but including those skilled in the art according to above detailed description it can be appreciated that it is modified, omit, example Such as any and whole embodiments of the combination between each embodiment, adaptive change and/or replacement.Restriction in claim It can widely be explained according to the language used in claim, and be not limited in foregoing detailed description or implementing to be somebody's turn to do The example described during application, these examples are considered as nonexcludability.It is in office where to arrange in method or process claims Any step lifted can in any order perform and be not limited to the order proposed in claim.Therefore, model of the invention Enclose only to be determined by appended claims and its legal equivalents, rather than by descriptions and examples given above Lai really It is fixed.

Claims (9)

  1. A kind of 1. preparation method of flue gas dearsenification adsorbent, it is characterised in that:By calcium oxide, metallurgical slag, zeolite and flyash Adsorbent is prepared after mixing and mixes material, then adsorbent is mixed in material addition cylindrical mixer adsorbent is prepared Particle.
  2. A kind of 2. preparation method of flue gas dearsenification adsorbent according to claim 1, it is characterised in that:Specific preparation side Method is:
    Step 1:Raw material mixing mixes
    Adsorbent is prepared in calcium oxide, metallurgical slag, zeolite and flyash after mixing and mixes material;
    Step 2:Granulation
    The adsorbent being prepared in step 1 is mixed material to add in cylindrical mixer, suction is prepared after the completion of mixing granulation Attached dose of particle;
    Step 3:Pretreatment
    The absorbent particles being prepared in step 2 are heated to 800-900 DEG C, adsorbent is obtained after the completion of cooling.
  3. A kind of 3. preparation method of flue gas dearsenification adsorbent according to claim 2, it is characterised in that:Step 1:Raw material What mixing mixed concretely comprises the following steps:
    (1) mixture A is prepared:Calcium oxide, metallurgical slag and zeolite are weighed by mass fraction to be added sequentially in mixer, are being stirred Mix and mixture A is made in machine after mixing;
    (2) flyash pre-processes:Flyash is added in sodium hydroxide solution, the concentration of sodium hydroxide solution is 1.5mol/ L, modified coal ash is obtained after dry;
    (3) flyash is added into mixture A, then additive is added in above-mentioned mixture again, after mixing Adsorbent is prepared and mixes material.
  4. A kind of 4. preparation method of flue gas dearsenification adsorbent according to claim 2, it is characterised in that:Step 3:Pre- place Reason concretely comprises the following steps:The absorbent particles being prepared in step 2 are placed into micro-wave oven, and in the bar of nitrogen protection Microwave heating is carried out under part, is heated to 800-900 DEG C, 30min is kept the temperature, adsorbent is obtained after the completion of cooling.
  5. A kind of 5. preparation method of flue gas dearsenification adsorbent according to claim 2, it is characterised in that:The addition of flyash Measure as M4=γ (M1+ α M2- δ M3)-β/(1- α) M2, wherein:M1 be calcium oxide quality, M2 be metallurgical slag quality, M3 For the quality of zeolite;It is CaO the and MgO mass percentages in metallurgical slag that γ, which takes 0.15~0.25, δ to take 1.5-2, α,;β is Fe in metallurgical slag2O3With MnO mass percentages.
  6. 6. according to a kind of preparation method of flue gas dearsenification adsorbent of claim 1-5 any one of them, it is characterised in that:Oxidation The mass ratio of calcium and metallurgical slag is 2.2~4.0.
  7. A kind of 7. preparation method of flue gas dearsenification adsorbent according to claim 6, it is characterised in that:Further include addition Agent, the additive include blast furnace ash, chromium slag and mullite.
  8. A kind of 8. preparation method of flue gas dearsenification adsorbent according to claim 7, it is characterised in that:The additive Addition be adsorbent 2-5%.
  9. A kind of 9. preparation method of flue gas dearsenification adsorbent according to claim 7, it is characterised in that:Further include promotion Agent, the accelerating agent are more than 1000 organic matter for draw ratio.
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