CN109908951A - A kind of micro--mesoporous low temperature catalyst of multistage and preparation method thereof - Google Patents
A kind of micro--mesoporous low temperature catalyst of multistage and preparation method thereof Download PDFInfo
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Abstract
The invention discloses micro--mesoporous low temperature catalyst of a kind of multistage and preparation method thereof, which is indicated by the following general formula (1), W-LaMnO3Wherein, in the general formula (1), HZSM-5-X is carrier to/HZSM-5-X ... general formula (1), and X indicates SiO2With Al2O3Ratio；W:La:Mn molar ratio is (0.2-0.25): 1:1.It uses solid waste coal ash to synthesize HZSM-5-X for main material extraction Si, Al, is reuse of solid waste.The W-LaMnO of synthesis3/ HZSM-5-X, specific surface area reach 320-417m2/ g has and resists organic sulfur and SO in exhaust gas2Poison characteristic, H in exhaust gas2O and W-LaMnO3/ HZSM-5-X forms Strong oxdiative object H5O2 +Promote VOCs oxidation.The catalyst temperature of preparation improves W-LaMnO at 240-300 DEG C of low temperature3The application range of/HZSM-5-X.
Description
Technical field
The present invention relates to catalyst technical field, more particularly to a kind of catalysis oxidation volatile organic matter multistage it is micro--
Mesoporous low temperature catalyst and preparation method thereof.
Background technique
Oil smoke is one of food processing and the most important atmosphere pollution of catering industry, and greasy fine particle partial size is in 20-
Between 100 nanometers, concentration may be up to 200 milligrams/cubic metre.Contain a large amount of volatilization/semi-volatile organic matter in oil smoke, mainly
There are the pollutants such as aldehyde, ketone, hydrocarbon, fatty acid, alcohol, aromatic compound, ester, lactone, heterocyclic compound, untreated oil smoke row
It puts and ambient air quality environment is caused to seriously affect, especially the larger organic matter of irritation taste, human body smell can be generated
Stronger sensitivity response, enterprise's nearby residents are complained more.
Existing oil smoke processing technology mainly includes conventional purge technology: alkali liquid washing, electrostatic treatment, UV photodissociation and active carbon
The technological means such as absorption.
Oil smoke and VOCs processing are big insufficient there are following three at present:
The first, conventional processing device is to oil smoke poor processing effect.The universal open system of oil smoke is collected, and system is collected excessive empty
Gas, oil flue waste gas amount is big, and subsequent processing device load is high, needs huge processing system.Oil smoke partial size is 20-100 nanometers
Superfine particulate matter exists in exhaust with aerosol form, and is insoluble in water, thus the purification efficiency of washing facility is limited, washes
It washs waste water and is also easy to produce secondary pollution.Grease concentration reaches as high as 20-100mg/m3 in oil smoke, and adhesiveness is strong, is easily adhered to pipe
On road, cleaning equipment (being separated by filtration, electrostatic, photodissociation etc.), cleaning equipment is caused to be difficult to continually and steadily run, it is oily in cleaning equipment
Rouge heavy workload.Filtering separation device extends with filtration time, and filtering layer resistance is gradually increased, and oil smoke treatment effect is deteriorated and filters
Expect cracky, because adsorbent material cleans difficulty, filtrate is difficult to reuse, and is also easy to produce secondary pollution when discarded individually disposition.
The second, conventional processing device is difficult to volatilization/Semi-volatile organism peculiar smell.Exist in oil flue waste gas and largely waves
Hair/Semi-volatile organism mainly has hydro carbons ((two) chloromethanes, dicholorodifluoromethane, chloroethanes, just oneself (heptan) alkane etc.), alkenes
(propylene, vinyl chloride, butadiene etc.), oxygen-bearing organic matter (ketone, aldehydes) etc., are the main sources of peculiar smell.Conventional purge technology
(washing, electrostatic, photodissociation etc.) is poor to the decomposition removal efficiency of organic matter.
Sulphur preferably makes catalyst poisoning in exhaust gas when third, catalysis burning.If when burning processing organic sulfur to oil smoke grease and
The burning processing of organic matter is most thorough and high-efficient, but because air quantity is big (separate unit cooking stove air quantity reaches 2000m3/h), volatilization/half
Low for volatile organic compounds concentration relative combustion, exhaust gas is directly catalyzed burning, and energy consumption is huge is difficult to realize；When cooking stove fuel is coke
When charcoal, the sulfur that coke burns when burning waste gas is mixed into oil smoke easily makes catalyst poisoning, reduces catalysis efficiency of combustion.
According to data consultation, VOCs oxidation catalyst and preparation method thereof has the following patent:
CN20181032724.1 discloses a kind of monoblock type VOCs oxidation catalyst and preparation method thereof.The monoblock type
VOCs oxidation catalyst includes carrier, is uniformly embedded into the carrier inside and the evenly distributed catalysis in the carrier
Evenly dispersed active component and auxiliary agent in agent coating and the catalyst coat, wherein the carrier is corrugation fiber paper base
Material rolls or is laminated the monoblock type corrugation fiber paper supports formed.
CN2017111787704.8 discloses a kind of VOCs catalyst for treating waste gas, and the catalyst is made with porous metals
For carrier, coating is coated on carrier；The coating includes that Pt compounding LaMnO3 Ca-Ti ore type meets oxide, with transition metal
One of element or a variety of manufactured solid solution, oxides are support modification agent, γ-Al2O3 powder.
CN201811080301.4 discloses a kind of VOCs catalyst for catalytic combustion material and preparation method thereof, the patent control
The amount ratio and preparation method technological parameter of each raw material are made, directly mixed, formed with manganese dioxide and other inorganic minerals, is burnt into
It is prepared into catalyst for catalytic combustion material.
The catalyst specific surface that the cost of material of the generally existing production carrier of the catalyst recorded in above-mentioned patent is high, is formed
Product is small to absorb the disadvantages of insufficient, catalytic temperature requires higher application range small.
Summary of the invention
The present invention provides micro--mesoporous low temperature catalysts of a kind of multistage and preparation method thereof.
The present invention provides following schemes:
A kind of micro--mesoporous low temperature catalyst of multistage, comprising:
It is indicated by the following general formula (1),
W-LaMnO3/ HZSM-5-X ... general formula (1)
Wherein, in the general formula (1), HZSM-5-X is carrier, and X indicates SiO2With Al2O3Ratio；W:La:Mn molar ratio
For (0.2-0.25): 1:1.
Preferably: the X=1:(0.5-3).
A kind of preparation method of micro--mesoporous low temperature catalyst of multistage, which comprises
SiO is extracted from flyash2And Al2O3, by the SiO of extraction2And Al2O3In proportion with Na2O, tetrapropyl hydrogen
Amine-oxides substep, which is mixed, is thermally formed gel；
The gel and polydimethyl diallyl ammonium chloride are mixed in proportion and obtain HZSM-5-X carrier；
By dipping method by La (NO3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is immersed in the HZSM-5-X carrier
In, temperature programming calcining prepares the W-LaMnO3/ HZSM-5-X catalyst.
Preferably: described that SiO is extracted from flyash2And Al2O3Include:
SiO will be extracted by leaching method after flyash and NaOH calcining2And Al2O3。
Preferably: by flyash 750-850 DEG C temperature lower calcination 2.2-2.6 hours, be then blended in 820- with NaOH
860 DEG C temperature lower calcination 2.5-3.2 hours, obtain calcined product；The calcined product is cooled to 46-55 DEG C of addition 3mol/L
HCl control liquid-solid ratio be 10:1, stirring obtains the colloidal sol for being rich in Si, Al substance for 2.5-3.2 hour；It adjusts PH and is passed through CO2
Filter separating, washing, drying obtains SiO2And Al2O3。
Preferably: the molar ratio of each substance is H in the gel2O:SiO2:Al2O3:Na2O: tetrapropylammonium hydroxide=
20:100:x:0.12:0.2；The X is SiO2With Al2O3Ratio.
Preferably: X=50,100,150,200,250,300.
Preferably: the gel being mixed in proportion with polydimethyl diallyl ammonium chloride and is obtained by hydrothermal synthesis preparation
Obtain HZSM-5-X carrier.
Preferably: the specific surface area of the HZSM-5-X carrier is 320-417m2/g。
Preferably: control W:La:Mn molar ratio is (0.2-0.25): 1:1, LaMnO3Weight accounting be 10%.
The specific embodiment provided according to the present invention, the invention discloses following technical effects:
By the invention it is possible to a kind of micro--mesoporous low temperature catalyst of multistage and preparation method thereof be realized, in a kind of realization side
Under formula, which is indicated by the following general formula (1), W-LaMnO3/ HZSM-5-X ... general formula (1) wherein, in the general formula (1),
HZSM-5-X is carrier, and X indicates SiO2With Al2O3Ratio；W:La:Mn molar ratio is (0.2-0.25): 1:1.It is useless using solid
Gurry flyash is that main material extraction Si, Al synthesizes HZSM-5-X, is reuse of solid waste.The W-LaMnO of synthesis3/
HZSM-5-X, specific surface area reach 320-417m2/ g has and resists organic sulfur and SO in exhaust gas2Poison characteristic, H in exhaust gas2O
With W-LaMnO3/ HZSM-5-X forms Strong oxdiative object H5O2 +Promote VOCs oxidation.The catalyst temperature of preparation is in low temperature
240-300 DEG C, improve W-LaMnO3The application range of/HZSM-5-X.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is SiO provided in an embodiment of the present invention2/Al2O3Ratio is to W-LaMnO3/ HZSM-5-X catalysis oxidation valeral
The first schematic diagram influenced；
Fig. 2 is SiO provided in an embodiment of the present invention2/Al2O3Ratio is to W-LaMnO3/ HZSM-5-X catalysis oxidation valeral
The second schematic diagram influenced；
Fig. 3 is 2vol.%H provided in an embodiment of the present invention2W-LaMnO under O humidity3/ HZSM-5-X catalysis oxidation valeral
First schematic diagram；
Fig. 4 is 2vol.%H provided in an embodiment of the present invention2W-LaMnO under O humidity3/ HZSM-5-X catalysis oxidation valeral
Second schematic diagram.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art's every other embodiment obtained belong to what the present invention protected
Range.
The embodiment of the invention provides a kind of micro--mesoporous low temperature catalysts of multistage, and the catalyst is by the following general formula (1) table
Show,
W-LaMnO3/ HZSM-5-X ... general formula (1)
Wherein, in the general formula (1), HZSM-5-X is carrier, and X indicates SiO2With Al2O3Ratio；W:La:Mn molar ratio
For (0.2-0.25): 1:1.
Wherein, the X=1:(0.5-3).
Catalyst W-LaMnO3The cryogenic temperature section of/HZSM-5-X catalysis oxidation volatile organic matter VOCs is 240-
00℃；H2O and W-LaMnO in exhaust gas3/ HZSM-5-X forms Strong oxdiative object H5O2 +, thus promote the oxidation of VOCs；To oil smoke
VOCs valeral (C5H10O oxygenation efficiency) is greater than 98%；Organic combustion of sulfur in organic exhaust gas can be resisted and generate SO2Poisoning.
The embodiment of the present application can also provide a kind of preparation method of micro--mesoporous low temperature catalyst of multistage, the side
Method includes:
From flyash extract SiO2 and Al2O3, by the SiO2 of extraction and Al2O3 in proportion with Na2O, tetrapropyl
Ammonium hydroxide substep, which is mixed, is thermally formed gel；Specifically, by being extracted after flyash and NaOH calcining by leaching method
SiO2And Al2O3.Further, by flyash 750-850 DEG C temperature lower calcination 2.2-2.6 hours, then mixed with NaOH
820-860 DEG C temperature lower calcination 2.5-3.2 hours, obtain calcined product；The calcined product is cooled to 46-55 DEG C of addition
The HCl control liquid-solid ratio of 3mol/L is 10:1, and stirring obtains the colloidal sol rich in Si, Al substance for 2.5-3.2 hours；It adjusts PH and leads to
Enter CO2Filter separating, washing, drying obtains SiO2And Al2O3.The molar ratio of each substance is H in the gel2O:
SiO2:Al2O3:Na2O: tetrapropylammonium hydroxide=20:100:x:0.12:0.2；The X is SiO2With Al2O3Ratio.X=
50,100,150,200,250,300。
The gel and polydimethyl diallyl ammonium chloride are mixed in proportion and obtain HZSM-5-X carrier；Specifically
, the gel is mixed in proportion with polydimethyl diallyl ammonium chloride, HZSM-5-X load is prepared by hydrothermal synthesis
Body.The specific surface area of the HZSM-5-X carrier is 320-417m2/g。
By dipping method by La (NO3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is immersed in the HZSM-5-X carrier
In, control W:La:Mn molar ratio is (0.2-0.25): 1:1, LaMnO3Weight accounting be 10%.Temperature programming calcining preparation
Obtain the W-LaMnO3/ HZSM-5-X catalyst.
This method is to extract SiO by leaching method after flyash and NaOH calcining2、Al2O3, then with Na2O、TPAOH
Substep is mixed and is thermally formed gel, and gel is mixed in proportion with polydimethyl diallyl ammonium chloride (PDADMAC) and is led to
Cross hydrothermal synthesis preparation HZSM-5-X carrier.Controlling W:La:Mn molar ratio is (0.2-0.25): 1:1, LaMnO3Weight accounting
It is 10%, by dipping method by La (NO3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is immersed in HZSM-5-X carrier, most
It is prepared into W-LaMnO eventually3/ HZSM-5-X catalyst.
The present invention has the advantages that
To achieve the above object, the present invention uses following technical method:
First, leaching method: flyash and NaOH being mixed in a certain ratio and calcined in certain temperature, and 3M HCl control is added
Liquid-solid ratio processed is that 10:1 obtains the colloidal sol for being rich in Si, Al substance, and adjusting PH is passed through CO2 and filters, separation, washing, dries acquisition richness
Containing Si, Al substance.
Second, hydrothermal synthesis method: controlling the ratio of SiO2/Al2O3, and heating shape is mixed with Na2O, TPAOH substep
At gel, gel is mixed in proportion with polydimethyl diallyl ammonium chloride (PDADMAC), HZSM- is prepared by hydrothermal synthesis
5-X carrier (X is the ratio of SiO2/Al2O3, X=50,100,150,200,250,300), specific surface area reaches 320-417m2/
g。
Third, dipping method: control W:La:Mn molar ratio is (0.2-0.25): the weight accounting of 1:1, LaMnO3 are
10%, La (NO3) 3, Mn (NO3) 2,3 (NH4) 2O-7WO3-6H2O are immersed in HZSM-5-X carrier, temperature programming calcining
Prepare W-LaMnO3/HZSM-5-X catalyst.
The present invention has the advantages that
It uses solid waste coal ash to synthesize HZSM-5-X for main material extraction Si, Al, is reuse of solid waste.
The W-LaMnO of synthesis3/ HZSM-5-X, specific surface area reach 320-417m2/ g has and resists organic sulfur and SO in exhaust gas2Poison
Change characteristic, H in exhaust gas2O and W-LaMnO3/ HZSM-5-X forms Strong oxdiative object H5O2 +Promote VOCs oxidation.The catalyst of preparation is urged
Change temperature at 240-300 DEG C of low temperature, improves W-LaMnO3The application range of/HZSM-5-X.
Catalyst mentioned below by specific embodiment to application and preparation method thereof carries out message introduction, following embodiment
In the source of each raw material is not particularly limited, be commercially available.
Embodiment 1
Firstly, extracting Si, Al in flyash.By flyash in 800 DEG C of calcining 2.5h, 850 DEG C are then mixed with NaOH and is forged
3h is burnt, 50 DEG C of addition 3M HCl stirring 2h is subsequently cooled to, obtains the precipitating for being rich in Si, Al, adjust PH=12.5 and obtain hydrogen
Aluminium oxide.In the precipitating rich in Si, appropriate NaOH80 DEG C of stirring 2h is added, is washed out and obtains SiO2、Al2O3。
Secondly, synthesis HZSM-5-X carrier.By the SiO of extraction2、Al2O3By different proportion and Na2O, TPAOH substep mixes
Agitating and heating forms gel, and the molar ratio of each substance is H in gel2O:SiO2:Al2O3:Na2O:TPAOH (tetrapropyl hydroxide
Ammonium)=20:100:x:0.12:0.2 (X SiO2/Al2O3Ratio, X=50,100,150,200,250,300).By gel with
Polydimethyl diallyl ammonium chloride (PDADMAC) mixes in proportion prepares HZSM-5-X carrier, specific surface by hydrothermal synthesis
Product reaches 320-417m2/g。
Finally, passing through dipping method for La (NO3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is immersed in HZSM-5-X load
In body, the molar ratio for controlling La:Mn:W is 1:1:0.2-0.25, temperature programming calcining preparation W-LaMnO3/ HZSM-5-X catalysis
Agent.
W-LaMnO3/HZSM-5-X (X=50,100,150,200,250and300) catalysis prepared by above-described embodiment 1
Agent, under 200 DEG C of air conditions of valeral (C5H10O) concentration 210ppm, catalytic efficiency is followed successively by W-LaMnO3/HZSM-5-
300<W-LaMnO3/HZSM-5-50<W-LaMnO3/HZSM-5-250<W-LaMnO3/HZSM-5-200<W-LaMnO3/HZSM-
5-150<W-LaMnO3/HZSM-5-100.With the progress of reaction, catalytic efficiency is first increased with the raising of SiO2/Al2O3 ratio
After reduce, in addition to W-LaMnO3/HZSM-5-300, W-LaMnO3/HZSM-5-X (X=50,100,150,200and 250) is right
The catalytic efficiency of valeral (C5H10O) is higher than 96%, as shown in Figure 1 and Figure 2.
W-LaMnO3/HZSM-5-X (X=50,100,150,200,250and 300) catalyst prepared in embodiment 1
Under the conditions of 2vol.%H2O, W-LaMnO3/HZSM-5-50 and W-LaMnO3/HZSM-5-100 urge valeral (C5H10O)
Change efficiency and reaches 100%.As SiO2/Al2O3 ratio increases, H2O reduces the facilitation of catalytic efficiency, but reduces amplitude
Within 5%, total catalytic efficiency is greater than 95%.As shown in Figure 3, Figure 4.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (10)
1. a kind of micro--mesoporous low temperature catalyst of multistage, which is characterized in that it is indicated by the following general formula (1),
W-LaMnO3/ HZSM-5-X ... general formula (1)
Wherein, in the general formula (1), HZSM-5-X is carrier, and X indicates SiO2With Al2O3Ratio；W:La:Mn molar ratio is
(0.2-0.25):1:1。
2. micro--mesoporous low temperature catalyst of multistage according to claim 1, which is characterized in that the X=1:(0.5-3).
3. a kind of preparation method of micro--mesoporous low temperature catalyst of multistage as claimed in claim 1 or 2, which is characterized in that the method
Include:
SiO is extracted from flyash2And Al2O3, by the SiO of extraction2And Al2O3In proportion with Na2O, tetrapropylammonium hydroxide
Substep is mixed and is thermally formed gel；
The gel and polydimethyl diallyl ammonium chloride are mixed in proportion and obtain HZSM-5-X carrier；
By dipping method by La (NO3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is immersed in the HZSM-5-X carrier,
Temperature programming calcining prepares the W-LaMnO3/ HZSM-5-X catalyst.
4. according to the method described in claim 3, it is characterized in that, described extract SiO from flyash2And Al2O3Include:
SiO will be extracted by leaching method after flyash and NaOH calcining2And Al2O3。
5. according to the method described in claim 4, it is characterized in that, by flyash in 750-850 DEG C of temperature lower calcination 2.2-2.6
Hour, it is then blended in 820-860 DEG C of temperature lower calcination with NaOH 2.5-3.2 hours, obtains calcined product；The calcining is produced
The HCl control liquid-solid ratio that object is cooled to 46-55 DEG C of addition 3mol/L is 10:1, and stirring is obtained rich in Si, Al object for 2.5-3.2 hours
The colloidal sol of matter；It adjusts PH and is passed through CO2Filter separating, washing, drying obtains SiO2And Al2O3。
6. according to the method described in claim 3, it is characterized in that, the molar ratio of each substance is H in the gel2O:SiO2:
Al2O3:Na2O: tetrapropylammonium hydroxide=20:100:x:0.12:0.2；The X is SiO2With Al2O3Ratio.
7. according to the method described in claim 6, it is characterized in that, X=50,100,150,200,250,300.
8. according to the method described in claim 3, it is characterized in that, the gel is pressed with polydimethyl diallyl ammonium chloride
Ratio mixing prepares HZSM-5-X carrier by hydrothermal synthesis.
9. according to the method described in claim 8, it is characterized in that, the specific surface area of the HZSM-5-X carrier is 320-
417m2/g。
10. according to the method described in claim 3, it is characterized in that, control W:La:Mn molar ratio be (0.2-0.25): 1:1,
LaMnO3Weight accounting be 10%.
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| CN110586176A (en) * | 2019-09-27 | 2019-12-20 | 中国环境科学研究院 | Electrolytic manganese slag-based micro-mesoporous ZSM-5 catalyst and preparation method thereof |
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