CN104785205B - A kind of Solid Modified complex type molecular sieve mercury removal agent and preparation method thereof - Google Patents
A kind of Solid Modified complex type molecular sieve mercury removal agent and preparation method thereof Download PDFInfo
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- CN104785205B CN104785205B CN201510187595.0A CN201510187595A CN104785205B CN 104785205 B CN104785205 B CN 104785205B CN 201510187595 A CN201510187595 A CN 201510187595A CN 104785205 B CN104785205 B CN 104785205B
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Abstract
The present invention relates to a kind of Solid Modified complex type molecular sieve mercury removal agent and preparation method thereof, complex type molecular sieve mercury removal agent of the present invention is mainly modified the molecular sieve with special skeleton structure using strong catalysis oxidation material, form compound mercury removal agent, selected framework of molecular sieve also has stronger demercuration performance in itself, and molecular sieve specific surface area is big, and heat endurance is good, high mechanical strength, it is the excellent carrier of strong catalysis oxidation material, abundant raw material can manually control synthesis；The complex type molecular sieve mercury removal agent can be in efficient removal flue gas mercury vapour, demercuration efficiency is high, process is simple, non-secondary pollution；Can be independently operated, easily can also be used in combination with existing cleaning equipment, and can reclaim reuse after mercury simple substance.
Description
Technical field
The present invention relates to a kind of mercury removal agent in exhaust-gas treatment field, specifically, it is related to a kind of Solid Modified compound
Molecular sieve mercury removal agent and preparation method thereof.
Background technology
The discharge of mercury and Environmental capacity are environmentally friendly focuses, and its steam is forced down, volatile, is global pollutant.It is wide
It is general to be present in air, water body, soil, and constantly circulated in the presence of natural force.Generally, the discharge of coal fired power plant mercury is dense
It is 0.1~0.6mg/m to spend3, and the concentration of junk discharged in burning mercury is then in 10~100mg/m3Between.With industrialize into
The acceleration of journey, the cumulant of mercury also constantly increases in air, seriously beyond the background value of mercury in the Nature.Both at home and abroad to flue gas
The research of demercuration is developed rapidly, but is made little progress at present, although researcher has attempted number of types of demercuration adsorbent,
But do not find that demercuration efficiency is high and economical, can be widely used in the mercury absorbent of industrial ideal type also so far, therefore continue
It is problem in the urgent need to address in waste gas pollution control and treatment to explore high-efficiency mercury removal agent.
In flue gas the removal methods of Elemental Mercury mainly include absorption method, using existing dust arrester or desulfurizer demercuration
Method, chemical oxidization method, metal and metal oxide and pulsed discharge plasma method etc..In recent years, using existing purification
Device realizes that demercuration is one of domestic and international popular research simultaneously.Adsorbent based on bag-type dusting and electrostatic precipitation sprays into technology
The emphasis studied both at home and abroad.Acticarbon is very high to each form mercury removal efficiency, up to more than 90%, and can take off simultaneously
Except the toxic gas of other species, but there is also the low shortcoming of large-scale use cost performance.Flying dust demercuration efficiency is unstable；Calcium base
Class material is low to Hg0 removal efficiencies, can only achieve 10%~20%；Gaseous cyaniding mainly realizes a Hg0Switch to Hg2+, efficiency
Height it is closely related with the gas componant to be aoxidized, it is simple to operate, but for aoxidize gas production rates it is low, prepare it is costly；
Hydroxyl radical free radical oxidation technology efficiency is higher, but the OH time-to-live is short, energy consumption is big, it is inefficient, be difficult for long-term stable operation.
Based on drawbacks described above and demand, taken off it is an object of the invention to provide a kind of efficient Solid Modified complex type molecular sieve
Mercurial.
The content of the invention
It is an object of the invention to provide a kind of Solid Modified complex type molecular sieve mercury removal agent and preparation method thereof.It is described compound
Type molecular sieve mercury removal agent can be in efficient removal flue gas mercury vapour, demercuration efficiency is high, process is simple, non-secondary pollution, and
Reused after mercury simple substance can be reclaimed.
Solid Modified complex type molecular sieve mercury removal agent of the present invention mainly make use of potassium ferrate (K2FeO4) strong oxygen
The property changed, nontoxicity, the ability combined with mercury.
Solid Modified complex type molecular sieve mercury removal agent of the present invention be molecular sieve with catalysis oxidation type material carry out from
Product after son exchange, is mainly prepared using following methods：By molecular sieve and K2FeO4Ion exchange is carried out, is obtained.
Wherein, the molecular sieve and K2FeO4Ion exchange process be Solid-state Ion-exchange process；Be by molecular sieve with
K2FeO4After mixing, being calcined 10-14h at 120-160 DEG C carries out Solid-state Ion-exchange；Wherein, the molecular sieve and K2FeO4Matter
Amount is than being 10:1.0-2.4.
Preferably, the molecular sieve and K2FeO4Mass ratio be 10:1.2-2.0.Wherein, the molecular sieve that the present invention is used
Can be various molecular sieves purchased in market, because molecular sieve inherently has good absorption property, it may have stronger demercuration
Can, and molecular sieve specific surface area is big, heat endurance is good, but it is preferable that the molecular sieve is through Materials Studio softwares
Simulation represents 145 kinds of molecular sieve adsorption Elemental Mercuries of different skeleton structures, filters out demercuration efficiency molecular sieve high.
It is furthermore preferred that the molecular sieve is the one kind in SOD, LTN, AEI, MFI.
Wherein, the SOD type molecule of the skeleton sieve typical material is sodalite, and its typical material composition is [Al6Si6O24],
But it is not limited to this composition.
The LTN types molecule of the skeleton sieve typical material composition is [Si384Al384O1536], but it is not limited to this composition.
The AEI types molecule of the skeleton sieve typical material composition is [Al24P24O96], but it is not limited to this composition.
The MFI-type molecular sieve is ZSM-5 molecular sieve, and typical material composition is [Si96O192], but it is not limited to this composition.
It is furthermore preferred that MFI type of the described molecular sieve for ZSM-5 molecular sieve, its micropore size 0.5-0.6nm；
In addition, the molecular sieve is before ion exchange, also including molecular sieve is purified, the purification is entered as follows
OK：Molecular sieve is ground, 300 mesh sieves are crossed, then molecular sieve is calcined at 120 DEG C -600 DEG C, it is miscellaneous in molecular sieve to remove
Matter, the molecular sieve being purified；
The roasting of the purifying step is preferably calcined 2h and carries out at 600 DEG C.
Further, it is the demercuration efficiency of raising complex type molecular sieve mercury removal agent, complex type molecular sieve of the present invention
Mercury removal agent before ion exchange is carried out, also including molecular sieve impregnated in into ammoniacal liquor in, then dry, be calcined；
Base extraction can change the pore volume and pore structure of molecular sieve, can optionally remove zeolitic frameworks silicon, improve de-
Mercury efficiency.
It is described molecular sieve be impregnated in into ammoniacal liquor in can carry out after the decontaminating step；
The results show, is impregnated using the ammoniacal liquor of various concentrations, can influence the complex type molecular sieve demercuration for preparing
The demercuration efficiency of agent, therefore, the concentration of the ammoniacal liquor is 0.5-3.0mol/L；The dip time is 6~8 hours.
Preferably, the concentration of the ammoniacal liquor is 1.0-3.0mol/L；The dip time is 6~8 hours.
The drying after ammoniacal liquor dipping is dried 3-8 hours to be placed in baking oven 100-150 DEG C；It is preferred that in 120 DEG C of dryings 6
Hour.
120 DEG C~600 DEG C are roasted to described in after ammoniacal liquor dipping to be calcined 2~6 hours；Preferable temperature is 300 DEG C, is preferably roasted
The burning time is 6 hours.
Described composite molecular screen mercury removal agent can be in efficient removal waste gas mercury, mercury removal agent is usually positioned over absorption anti-
Answer on bed, allow the air for carrying mercury vapour to pass through mercury removal agent；It is demonstrated experimentally that K2FeO4 modified molecular sieve demercuration efficiency is up to
85.3%.
Composite molecular screen mercury removal agent of the present invention can be recycled, and the molecular sieve mercury removal agent after the completion of demercuration can pass through
Heating collect Elemental Mercury, then by molecular sieve again with K2FeO4Carry out ion exchange, the ion exchange process with for the first time from
Sub- exchange process is identical, obtains the complex type molecular sieve mercury removal agent that can be reused.
Therefore, the present invention also provides the preparation method of above-mentioned complex type molecular sieve mercury removal agent.
The preparation method of complex type molecular sieve mercury removal agent of the present invention, comprises the following steps：
1) by molecular sieve and K2FeO4Ion exchange is carried out, complex type molecular sieve mercury removal agent is obtained.
Step 1) in, the molecular sieve and K2FeO4Ion exchange process be Solid-state Ion-exchange process；It is by molecular sieve
With K2FeO4After mixing, being calcined 10-14h at 120-160 DEG C carries out Solid-state Ion-exchange；Wherein, the molecular sieve and K2FeO4's
Mass ratio is 10:1.0-2.4；
The molecular sieve and K2FeO4Mass ratio preferably 10:1.2-2.0.
Wherein, the molecular sieve can be various molecular sieves purchased in market, because molecular sieve inherently has absorption well
Performance, it may have stronger demercuration performance, and molecular sieve specific surface area is big, heat endurance is good, but it is preferable that the molecular sieve is
145 kinds of molecular sieve adsorption Elemental Mercuries of different skeleton structures are represented through the simulation of Materials Studio softwares, demercuration is filtered out
The molecular sieve of efficiency high.
Preferably, the molecular sieve is that skeleton structure is the one kind in SOD, LTN, AEI, MFI-type molecular sieve；
Wherein, the SOD type molecule of the skeleton sieve typical material is sodalite, and its typical material composition is [Al6Si6O24],
But it is not limited to this composition.
The LTN types molecule of the skeleton sieve typical material composition is [Si384Al384O1536], but it is not limited to this composition.
The AEI types molecule of the skeleton sieve typical material composition is [Al24P24O96], but it is not limited to this composition.
The MFI-type molecular sieve is ZSM-5 molecular sieve, and typical material composition is [Si96O192], but it is not limited to this composition.
More preferably MFI type ZSM-5 molecular sieve, its micropore size 0.5-0.6nm.
Method of the present invention, in step 1) before, also including 1 ') purification molecular sieve：Molecular sieve is ground, 300 are crossed
Mesh sieve, is then calcined to molecular sieve at 120 DEG C -600 DEG C, to remove the impurity in molecular sieve, the molecular sieve being purified.
Step 1 ') in, the roasting preferable temperature is 300 DEG C, and preferably roasting time is 6 hours.
In addition, the ion-exchange effect to improve molecular sieve, method of the present invention, in step 1) before, also include
1 " during molecular sieve) impregnated in into ammoniacal liquor, then dry, be calcined；
Step 1 ") in, the concentration of the ammoniacal liquor is 0.5-3.0mol/L；The dip time is 6~8 hours.
Preferably, the concentration of the ammoniacal liquor is 1.0-3.0mol/L.
Step 1 ") in, the drying is dried 3-8 hours to be placed in baking oven 100-150 DEG C；It is preferred that small in 120 DEG C of dryings 6
When.
Step 1 ") in, it is described be roasted to 120 DEG C~600 DEG C be calcined 2~6 hours；Preferable temperature is 300 DEG C, is preferably calcined
Time is 6 hours.
The step 1 ') can be in step 1 ") carry out before.
Composite molecular screen mercury removal agent of the present invention can be recycled, therefore, preparation method of the present invention, in step
It is rapid 1) to include afterwards：Molecular sieve mercury removal agent after the completion of demercuration can collect Elemental Mercury by heating, then by molecular sieve
Again with K2FeO4Ion exchange is carried out, ion exchange process now is identical with the ion exchange process of first time, obtaining can be with
The complex type molecular sieve mercury removal agent for reusing.
Specifically, the preparation method of complex type molecular sieve mercury removal agent of the present invention, comprises the following steps：
1 ') molecular sieve purification：By ground 300 mesh sieve of molecular sieve, molecular sieve is calcined at 120 DEG C -600 DEG C, obtained
The ZSM-5 molecular sieve of purification；
1 " molecular sieve) be impregnated in into the hydration ammonia (NH that concentration is 0.5mol/L-3.0mol/L3·H2O), 6~8 hours,
Taking-up is put into baking oven 120 DEG C of dryings 6 hours, is subsequently placed in Muffle furnace and is calcined 2~6 hours in 120 DEG C~600 DEG C；
1) by molecular sieve and K2FeO4Ion exchange is carried out, compound mercury removal agent is obtained, wherein the molecular sieve and K2FeO4
Ion exchange process be Solid-state Ion-exchange process；It is by molecular sieve and K2FeO4After mixing, 10- is calcined at 120-160 DEG C
14h carries out Solid-state Ion-exchange；Wherein, the molecular sieve and K2FeO4Mass ratio be 10:1.0-2.4；It is preferred that 10:1.2-
2.0。
Wherein, the molecular sieve is the one kind in skeleton structure code SOD, LTN, AEI, MFI molecular sieve.
In addition, described preparation method, in step 1) after also include：2) recovery of complex type molecular sieve：It is compound
After the reaction of ZSM-5 molecular sieve mercury removal agent demercuration, intensification heating is carried out in special container, 120 DEG C -300 DEG C of heating-up temperature is reclaimed
Elemental Mercury, the molecular sieve for obtaining is ion-exchangeable, standby.
Compared with existing mercury removal agent, complex type molecular sieve mercury removal agent of the present invention mainly applies strong catalytic oxide
Matter is modified the molecular sieve with special skeleton structure, forms compound mercury removal agent, and selected framework of molecular sieve also has stronger in itself
Demercuration performance, and molecular sieve specific surface area is big, and heat endurance is good, high mechanical strength, is the excellent load of strong catalysis oxidation material
Body, abundant raw material can manually control synthesis, the complex type molecular sieve mercury removal agent can be in efficient removal flue gas mercury vapour,
Demercuration efficiency is high, process is simple, non-secondary pollution, and can reclaim reuse after mercury simple substance, and can be independently operated, also can be square
Just it is used in combination with existing cleaning equipment.
Specific embodiment
Below by specific embodiment in detail technical solution of the invention is described in detail, but protection scope of the present invention is not limited to down
The embodiment stated.
Wherein, each embodiment sets up demercuration experimental system, simulated flue gas generating means by the air as Balance Air, take
Air composition with mercury vapour.Its specific setting is as follows：
The air mass flow 200ml/min of mercury vapour is carried in duty parameter, is 800ml/ as the air mass flow of Balance Air
min；Mercury permeability 500ng/min (63 DEG C).Water vapor concentration is controlled by the speed of syringe pump propulsion water, advances speed
It is set to 10ml/min.
Mercury removal agent is positioned on adsorption reaction bed, allows the air for carrying mercury vapour to pass through mercury removal agent.
Embodiment 1
First weigh 100g MFI type ZSM-5 (silica alumina ratio is 50) molecular sieve be put into the roasting 2 hours of 600 DEG C of Muffle furnace after take
Go out, to remove the impurity of ZSM-5 molecular sieve trace, exclude the influence to subsequent experimental.
9 parts are weighed again through 600 DEG C of ZSM-5 molecular sieves of roasting, every part of quality is 10g, by 8 parts therein respectively with quality
It is 1.0g, the K of 1.2g, 1.4g, 1.6g, 1.8g, 2.0g, 2.2g, 2.4g2FeO4Solid-state Ion-exchange is carried out, is sufficiently mixed uniform
After be put into 150 DEG C of Muffle furnace, 12 hours of roasting after, cooling is taken out stand-by.
Take baked each 4g of ZSM-5 molecular sieve mercury removal agent, the successive reaction under the conditions of 30 DEG C under the conditions of 150 DEG C
80min, determines through different quality concentration K2FeO4(0.0g, 1.0g, 1.2g, 1.4g, 1.6g, 1.8g, 2.0g, 2.2g, 2.4g) changes
Property ZSM-5 molecular sieve mercury removal agent correspondence absorbing liquid concentration, and calculate demercuration efficiency and be respectively 55.6%, 58.8%,
65.5%, 66.48%, 68.52%, 63.1%, 57.78%, 50.6%, 49.86%.
Embodiment 2
First weigh 100g MFI type ZSM-5 (silica alumina ratio is 50) molecular sieve be put into the roasting 2 hours of 600 DEG C of Muffle furnace after take
Go out, to remove the impurity of ZSM-5 molecular sieve trace, exclude the influence to subsequent experimental.
Weigh again through 600 DEG C of ZSM-5 molecular sieve 10g of roasting, be the K of 1.6g with quality2FeO4Carry out solid ion friendship
Change, after 150 DEG C of 12 hours of roasting of Muffle furnace are put into after being sufficiently mixed uniformly, cooling is taken out stand-by.
The baked ZSM-5 molecular sieve mercury removal agent 4g under the conditions of 150 DEG C is taken, is reacted under the conditions of 80 DEG C, continuously
Reaction 120min, a concentration for absorbing liquid is determined every 10min, and calculates the removal efficiency of Elemental Mercury, 10min, 20min,
The different adsorption times of 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min
Corresponding demercuration efficiency is respectively 84.5%, 85.3%, 84.0%, 83.2%, 83.1%, 83.2%, 80.5%, 77.5%,
75.2%, 57.0%, 48.5%, 47.3%.
The ammoniacal liquor of embodiment 3 impregnates the influence to demercuration efficiency
First weigh after 100g molecular sieves are put into the roasting 2 hours of 600 DEG C of Muffle furnace and take out, to remove the miscellaneous of molecular sieve trace
Matter, excludes the influence to subsequent experimental.
Then ammoniacal liquor dipping experiment is carried out, is dried, is calcined.
10 parts of the ZSM-5 molecular sieve that 4g has removed impurity is taken, respectively the one of various concentrations (0.5mol/L-6.0mol/L)
Hydration ammonia (NH3·H2O dipping 6~8 hours in), taking-up is put into baking oven 120 DEG C of dryings 6 hours, be subsequently placed in Muffle furnace in
120 DEG C~600 DEG C are calcined 2~6 hours；After reacting 10min respectively under the conditions of 30 DEG C, its adsorption efficiency is determined, as a result such as table 1
It is shown.
The ammoniacal liquor of table 1 impregnates the influence to demercuration efficiency
In addition, by the impregnated molecular sieve of ammoniacal liquor and K2FeO4Ion exchange is carried out, the process of ion exchange is shown in embodiment 1,
Then demercuration experiment (reacting 10min respectively under the conditions of 30 DEG C) being carried out again, as a result being found, its demercuration efficiency averagely improves
15.0%.
Obviously, ammoniacal liquor dipping can improve demercuration efficiency.
Claims (10)
1. a kind of complex type molecular sieve mercury removal agent, it is characterised in that mainly prepared using following methods：By molecular sieve and K2FeO4
Solid-state Ion-exchange is carried out, is obtained；The Solid-state Ion-exchange is by molecular sieve and K2FeO4After mixing, in 120-160 DEG C of roasting
10-14h carries out Solid-state Ion-exchange；Wherein, the molecular sieve and K2FeO4Mass ratio be 10:1.0-2.4.
2. complex type molecular sieve mercury removal agent as claimed in claim 1, it is characterised in that the molecular sieve and K2FeO4Quality
Than being 10:1.2-2.0.
3. complex type molecular sieve mercury removal agent as claimed in claim 1 or 2, it is characterised in that the molecular sieve be SOD, LTN,
One kind in AEI, MFI；Wherein described LTN types molecule of the skeleton sieve typical material composition is [Si384Al384O1536]。
4. complex type molecular sieve mercury removal agent as claimed in claim 1, it is characterised in that the molecular sieve ion exchange it
Before, also including molecular sieve is purified, the purification is carried out as follows：Molecular sieve is ground, is sieved, then molecular sieve is existed
1-10h is calcined at 120 DEG C -600 DEG C, the molecular sieve being purified.
5. the complex type molecular sieve mercury removal agent as described in claim 1 or 4, it is characterised in that described complex type molecular sieve takes off
Mercurial before ion exchange is carried out, also including molecular sieve impregnated in into ammoniacal liquor in, then dry, be calcined；Wherein, the ammoniacal liquor
Concentration be 0.5-3.0mol/L；The dip time is 6~8 hours.
6. the preparation method of the complex type molecular sieve mercury removal agent as described in claim 1,4 and 5 are any, it is characterised in that including
Following steps：
1) by molecular sieve and K2FeO4Ion exchange is carried out, complex type molecular sieve mercury removal agent is obtained；
Wherein, the molecular sieve and K2FeO4Ion exchange process be Solid-state Ion-exchange process；The Solid-state Ion-exchange mistake
Journey is by molecular sieve and K2FeO4After mixing, being calcined 10-14h at 120-160 DEG C carries out Solid-state Ion-exchange；Wherein, the molecule
Sieve and K2FeO4Mass ratio be 10:1.0-2.4.
7. preparation method as claimed in claim 6, it is characterised in that in step 1) before, also including 1 ') purification molecular sieve：
Molecular sieve is ground, is sieved, 1-10h then is calcined at 120 DEG C -600 DEG C to molecular sieve, to remove the impurity in molecular sieve,
The molecular sieve being purified.
8. preparation method as claimed in claims 6 or 7, it is characterised in that in step 1) before, also including 1 ") by molecular sieve
Impregnated in ammoniacal liquor, then dry, be calcined.
9. preparation method as claimed in claims 6 or 7, it is characterised in that comprise the following steps：
1 ') molecular sieve purification：By ground 300 mesh sieve of molecular sieve, molecular sieve is calcined at 120 DEG C -600 DEG C, be purified
ZSM-5 molecular sieve；
1 " molecular sieve) be impregnated in into the hydration ammonia (NH that concentration is 0.5mol/L-3.0mol/L3·H2O), 6~8 hours, take out
120 DEG C of dryings 6 hours are put into baking oven, are subsequently placed in Muffle furnace and are calcined 2~6 hours in 120 DEG C~600 DEG C；
1) by molecular sieve and K2FeO4Ion exchange is carried out, compound mercury removal agent is obtained, wherein the molecular sieve and K2FeO4From
Sub- exchange process is Solid-state Ion-exchange process；It is by molecular sieve and K2FeO4After mixing, it is calcined 10-14h at 120-160 DEG C and enters
Row Solid-state Ion-exchange；Wherein, the molecular sieve and K2FeO4Mass ratio be 10:1.0-2.4.
10. preparation method as claimed in claim 9, it is characterised in that step 1) in, the molecular sieve and K2FeO4Quality
Than being 10:1.2-2.0.
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| CN101954241A (en) * | 2010-09-16 | 2011-01-26 | 宁波工程学院 | Method and device for removing odorous gas |
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| CN101954241A (en) * | 2010-09-16 | 2011-01-26 | 宁波工程学院 | Method and device for removing odorous gas |
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| Title |
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| New insights into synergistic effects and active species toward Hg0 emission control by Fe(VI) absorbent;Yinghui Han等;《Fuel》;20141011;第140卷;第309-316页 * |
| 高铁酸钾氧化-沸石吸附联合处理垃圾渗滤液;肖瑜等;《桂林理工大学学报》;20110228;第31卷(第1期);第123-127页 * |
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