CN109908951B - Multi-stage micro-mesoporous low-temperature catalyst and preparation method thereof - Google Patents
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Abstract
The invention discloses a multi-stage micro-mesoporous low-temperature catalyst and a preparation method thereof, wherein the catalyst is represented by the following general formula (1), W-LaMnO3The general formula (1) is shown in the specification, wherein in the general formula (1), HZSM-5-X is a carrier, and X represents SiO2With Al2O3The ratio of the molar ratios; the molar ratio of W to La to Mn is (0.2-0.25) to 1: 1. The solid waste fly ash is used as a main material to extract Si and Al to synthesize HZSM-5-X, and the solid waste is recycled. Synthetic W-LaMnO3HZSM-5-X, the specific surface area reaches 320-417m2G, having a resistance to organic sulfur and SO in exhaust gases2Poisoning property of, H in exhaust gas2O and W-LaMnO3Formation of Strong oxide H from/HZSM-5-X5O2 +Promoting the oxidation of VOCs. The catalytic temperature of the prepared catalyst is increased to 240 ℃ and 300 ℃ at low temperature, and the W-LaMnO content is increased3The application range of/HZSM-5-X.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a multistage micro-mesoporous low-temperature catalyst for catalytic oxidation of volatile organic compounds and a preparation method thereof.
Background
The oil fume is one of the most main atmospheric pollutants in the food processing and catering industries, the particle size of fine oily particles is between 20 and 100 nanometers, and the concentration can reach 200 mg/cubic meter. The oil fume contains a large amount of volatile/semi-volatile organic compounds, mainly pollutants such as aldehydes, ketones, hydrocarbons, fatty acids, alcohols, aromatic compounds, esters, lactones, heterocyclic compounds and the like, and untreated oil fume emission has serious influence on the surrounding air quality environment, particularly organic compounds with larger pungent taste can generate stronger sensitive reaction on the human smell, and the surrounding residents of enterprises have more complaints.
The existing oil smoke treatment technology mainly comprises the following traditional purification technologies: alkali liquor washing, electrostatic treatment, UV photolysis, active carbon adsorption and the like.
The prior oil smoke and VOCs treatment has the following three defects:
first, conventional treatment facility is poor to the oil smoke treatment effect. Oil smoke is collected by an open system generally, the system collects excessive air, the amount of oil smoke waste gas is large, the load of subsequent treatment equipment is high, and a huge treatment system is needed. Ultrafine particles with the oil smoke particle size of 20-100 nanometers exist in the form of aerosol in exhaust gas and are insoluble in water, so that the ultrafine particles are washedThe purification efficiency of the equipment is limited, and the washing wastewater is easy to generate secondary pollution. The oil concentration in the oil fume can reach 20-100mg/m at most3The grease cleaning agent has strong adhesion, is very easy to adhere to pipelines and purifying equipment (such as filtration separation, static electricity, photolysis and the like), leads the purifying equipment to be difficult to continuously and stably operate, and has large workload for cleaning the grease in the equipment. The filtering separation equipment has the advantages that the resistance of the filtering layer is gradually increased along with the prolonging of the filtering time, the oil smoke treatment effect is worsened, the filtering material is easy to damage, the filtering material is difficult to reuse due to the difficulty in cleaning the adsorbing material, and secondary pollution is easily caused when the waste is separately treated.
And secondly, the odor of the volatile/semi-volatile organic matters is difficult to treat by conventional treatment equipment. The oil fume exhaust contains a large amount of volatile/semi-volatile organic compounds, mainly hydrocarbons (methane chloride, dichlorodifluoromethane, chloroethane, n-hexyl (heptyl) alkane and the like), alkenes (propylene, vinyl chloride, butadiene and the like), oxygen-containing organic compounds (ketones, aldehydes) and the like, and the volatile/semi-volatile organic compounds are main sources of peculiar smell. The traditional purification technology (washing, static electricity, photolysis, etc.) has poor decomposition and removal efficiency on organic matters.
Thirdly, sulfur in the exhaust gas during catalytic combustion should poison the catalyst. If organic sulfur is used for completely burning oil fume, grease and organic matters during burning treatment and the burning treatment efficiency is high, but because the air volume is large (the air volume of a single stove reaches 2000m3/h), the concentration of volatile/semi-volatile organic matters is low relative to burning, and the direct catalytic burning of waste gas is huge and difficult to realize; when the fuel of the stove is coke, the sulfur burnt by the coke easily poisons the catalyst when the burning waste gas is mixed with the oil smoke, and the catalytic combustion efficiency is reduced.
According to the data, the following patents exist for the oxidation catalyst of VOCs and the preparation method thereof:
CN20181032724.1 discloses an integral VOCs oxidation catalyst and a preparation method thereof. The integral VOCs oxidation catalyst comprises a carrier, a catalyst coating which is uniformly embedded into the carrier and uniformly distributed on the surface of the carrier, and an active component and an auxiliary agent which are uniformly dispersed in the catalyst coating, wherein the carrier is an integral corrugated fiber paper carrier formed by rolling or laminating corrugated fiber paper base materials.
CN2017111787704.8 discloses that VOCs is uselessThe gas treatment catalyst takes porous metal as a carrier, and the carrier is coated with a coating; the coating comprises Pt compounded LaMnO3Perovskite type composite oxide, solid solution oxide prepared from one or more transition metal elements as a carrier modifier, and gamma-Al2O3And (3) powder.
CN201811080301.4 discloses a catalytic combustion catalyst material for VOCs and a preparation method thereof, the patent controls the dosage ratio of each raw material and the technological parameters of the preparation method, and manganese dioxide and other inorganic minerals are directly mixed, molded and sintered to form the catalytic combustion catalyst material.
The catalysts described in the above patents generally have the disadvantages of high raw material cost for preparing the carrier, small specific surface area of the formed catalyst, insufficient absorption, high catalytic temperature requirement, and small application range.
Disclosure of Invention
The invention provides a multi-stage micro-mesoporous low-temperature catalyst and a preparation method thereof.
The invention provides the following scheme:
a multi-stage micro-mesoporous low temperature catalyst comprising:
represented by the following general formula (1),
W-LaMnO3/HZSM-5-X … general formula (1)
Wherein in the general formula (1), HZSM-5-X is a carrier, and X represents SiO2With Al2O3The ratio of the molar ratio, wherein X is 50-300; the molar ratio of W to La to Mn is (0.2-0.25) to 1: 1.
A method for preparing a multi-stage micro-mesoporous low temperature catalyst, the method comprising:
extraction of SiO from fly ash2And Al2O3Extracting SiO2And Al2O3Proportionally with Na2Mixing O and tetrapropylammonium hydroxide step by step, stirring and heating to form gel;
mixing the gel and poly dimethyl diallyl ammonium chloride in proportion to prepare an HZSM-5-X carrier;
la (NO) by impregnation method3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is impregnated in the HZSM-5-X carrier, and the W-LaMnO is prepared by temperature programming and calcination3The catalyst is/HZSM-5-X catalyst.
Preferably: the SiO is extracted from the fly ash2And Al2O3The method comprises the following steps:
calcining fly ash and NaOH, and extracting SiO by leaching method2And Al2O3。
Preferably: calcining the fly ash at the temperature of 750-850 ℃ for 2.2-2.6 hours, and then mixing the fly ash with NaOH at the temperature of 820-860 ℃ for 2.5-3.2 hours to obtain a calcined product; cooling the calcined product to 46-55 ℃, adding 3mol/L HCl to control the liquid-solid ratio to be 10:1, and stirring for 2.5-3.2 hours to obtain sol rich in Si and Al substances; adjusting the pH and introducing CO2Filtering, separating, washing and drying to obtain SiO2And Al2O3。
Preferably: the molar ratio of each substance in the gel is H2O:SiO2:Al2O3:Na2Tetrapropylammonium hydroxide 20:100: x:0.12: 0.2.
Preferably: and mixing the gel and poly dimethyl diallyl ammonium chloride in proportion, and performing hydrothermal synthesis to obtain the HZSM-5-X carrier.
Preferably: the specific surface area of the HZSM-5-X carrier is 320-417m2/g。
Preferably: controlling the molar ratio of W to La to Mn to be (0.2-0.25):1:1, LaMnO3Is 10% by weight.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
by the invention, a multi-stage micro-mesoporous low-temperature catalyst and a preparation method thereof can be realized, and in one realization mode, the catalyst is represented by the following general formula (1), W-LaMnO3The general formula (1) is shown in the specification, wherein in the general formula (1), HZSM-5-X is a carrier, and X represents SiO2With Al2O3The ratio of the molar ratio, wherein X is 50-300; w is La:the molar ratio of Mn is (0.2-0.25) to 1: 1. The solid waste fly ash is used as a main material to extract Si and Al to synthesize HZSM-5-X, and the solid waste is recycled. Synthetic W-LaMnO3HZSM-5-X, the specific surface area reaches 320-417m2G, having a resistance to organic sulfur and SO in exhaust gases2Poisoning property of, H in exhaust gas2O and W-LaMnO3Formation of Strong oxide H from/HZSM-5-X5O2 +Promoting the oxidation of VOCs. The catalytic temperature of the prepared catalyst is increased to 240 ℃ and 300 ℃ at low temperature, and the W-LaMnO content is increased3The application range of/HZSM-5-X.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a SiO solid provided by an embodiment of the present invention2/Al2O3Proportional ratio W-LaMnO3A first schematic of the effect of/HZSM-5-X catalytic oxidation of valeraldehyde;
FIG. 2 shows SiO2/Al2O3Proportional ratio W-LaMnO3A second schematic of the effect of/HZSM-5-X catalytic oxidation of valeraldehyde;
FIG. 3 is a 2 vol.% H representation provided by an embodiment of the present invention2W-LaMnO at O humidity3A first schematic of/HZSM-5-X catalytic oxidation of valeraldehyde;
FIG. 4 is a 2 vol.% H representation provided by an embodiment of the present invention2W-LaMnO at O humidity3Second scheme of/HZSM-5-X catalytic oxidation of valeraldehyde.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
The embodiment of the invention provides a multi-stage micro-mesoporous low-temperature catalyst, which is represented by the following general formula (1),
W-LaMnO3/HZSM-5-X … general formula (1)
Wherein in the general formula (1), HZSM-5-X is a carrier, and X represents SiO2With Al2O3The ratio of the molar ratio, wherein X is 50-300; the molar ratio of W to La to Mn is (0.2-0.25) to 1: 1.
The catalyst W-LaMnO3The low-temperature interval of the/HZSM-5-X catalytic oxidation volatile organic compounds VOCs is 240-300 ℃; h in the exhaust gas2O and W-LaMnO3Formation of Strong oxide H from/HZSM-5-X5O2 +Thereby promoting oxidation of the VOCs; for oil smoke VOCs valeraldehyde (C)5H10O) oxidation rate is more than 98 percent; can resist SO generated by organic sulfur combustion in organic waste gas2Poisoning of (2).
The embodiment of the present application may further provide a preparation method of the multistage micro-mesoporous low temperature catalyst, where the method includes:
extraction of SiO from fly ash2And Al2O3Extracting SiO2And Al2O3Proportionally with Na2Mixing O and tetrapropylammonium hydroxide step by step, stirring and heating to form gel; specifically, the fly ash and NaOH are calcined and then extracted into SiO by a leaching method2And Al2O3. Further, calcining the fly ash at the temperature of 750-850 ℃ for 2.2-2.6 hours, and then mixing the fly ash with NaOH at the temperature of 820-860 ℃ for 2.5-3.2 hours to obtain a calcined product; cooling the calcined product to 46-55 ℃, adding 3mol/L HCl to control the liquid-solid ratio to be 10:1, and stirring for 2.5-3.2 hours to obtain sol rich in Si and Al substances; adjusting the pH and introducing CO2Filtering, separating, washing and drying to obtain SiO2And Al2O3. The substances in the gelIn a molar ratio of H2O:SiO2:Al2O3:Na2O tetrapropylammonium hydroxide-20: 100: X:0.12: 0.2; x is SiO2With Al2O3The ratio of (a) to (b). And X is 50,100,150,200,250,300.
Mixing the gel and poly dimethyl diallyl ammonium chloride in proportion to prepare an HZSM-5-X carrier; specifically, the HZSM-5-X carrier is prepared by mixing the gel and the poly dimethyl diallyl ammonium chloride in proportion and performing hydrothermal synthesis. The specific surface area of the HZSM-5-X carrier is 320-417m2/g。
La (NO) by impregnation method3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is impregnated in the HZSM-5-X carrier, the molar ratio of W to La to Mn is controlled to be (0.2-0.25):1:1, and LaMnO is controlled3Is 10% by weight. Preparing the W-LaMnO by temperature programming and calcination3The catalyst is/HZSM-5-X catalyst.
The method uses the method of extracting SiO by leaching after calcining fly ash and NaOH2、Al2O3Then with Na2O, TPAOH mixing, stirring, heating to form gel, mixing the gel with poly dimethyl diallyl ammonium chloride (PDADMAC) in proportion, and preparing HZSM-5-X carrier by hydrothermal synthesis. Controlling the molar ratio of W to La to Mn to be (0.2-0.25):1:1, LaMnO3Is 10%, and La (NO) is impregnated by the impregnation method3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is dipped in the HZSM-5-X carrier to prepare W-LaMnO finally3The catalyst is/HZSM-5-X catalyst.
The invention has the advantages that:
in order to achieve the purpose, the invention adopts the following technical method:
first, the leaching method: mixing fly ash and NaOH according to a certain proportion, calcining at a certain temperature, adding 3MHCl to control the liquid-solid ratio to be 10:1 to obtain sol rich in Si and Al, adjusting PH, and introducing CO2Filtering, separating, washing and drying to obtain Si and Al-rich substances.
Secondly, a hydrothermal synthesis method comprises the following steps: control of SiO2/Al2O3In a ratio of Na2O, TPAOH mixing, stirring, heating to form gel, mixing the gel with poly dimethyl diallyl ammonium chloride (PDADMAC) at a certain proportion, and hydrothermal synthesizing to obtain HZSM-5-X carrier (X is SiO)2/Al2O3X-50,100,150,200,250,300), the specific surface area reaches 320-2/g。
Thirdly, the dipping method: controlling the molar ratio of W to La to Mn to be (0.2-0.25):1:1, LaMnO3Is 10% by weight of La (NO)3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2Soaking O in HZSM-5-X carrier, and calcining at programmed temperature to prepare W-LaMnO3The catalyst is/HZSM-5-X catalyst.
The invention has the advantages that:
the solid waste fly ash is used as a main material to extract Si and Al to synthesize HZSM-5-X, and the solid waste is recycled. Synthetic W-LaMnO3HZSM-5-X, the specific surface area reaches 320-417m2G, having a resistance to organic sulfur and SO in exhaust gases2Poisoning property of, H in exhaust gas2O and W-LaMnO3Formation of Strong oxide H from/HZSM-5-X5O2 +Promoting the oxidation of VOCs. The catalytic temperature of the prepared catalyst is increased to 240 ℃ and 300 ℃ at low temperature, and the W-LaMnO content is increased3The application range of/HZSM-5-X.
The catalyst and the preparation method thereof are described below in detail by way of specific examples, and the sources of the raw materials in the following examples are not particularly limited and may be commercially available.
Example 1
Firstly, Si and Al in the fly ash are extracted. Calcining the fly ash at 800 ℃ for 2.5h, mixing the calcined fly ash with NaOH at 850 ℃ for 3h, cooling to 50 ℃, adding 3M HCl, stirring for 2h to obtain a precipitate rich in Si and Al, and adjusting the pH value to 12.5 to obtain the aluminum hydroxide. Adding a proper amount of NaOH into the precipitate rich in Si, stirring for 2h at 80 ℃, and then washing to obtain SiO2、Al2O3。
Next, HZ is synthesizedSM-5-X vector. Extracting SiO2、Al2O3In different proportions with Na2O, TPAOH mixing, stirring and heating step by step to form gel, wherein the molar ratio of each substance in the gel is H2O:SiO2:Al2O3:Na2TPAOH (tetrapropylammonium hydroxide) ═ 20:100: X:0.12:0.2(X is SiO)2/Al2O3Molar ratio, X-50,100,150,200,250,300). Mixing the gel and poly dimethyl diallyl ammonium chloride (PDADMAC) in proportion, and preparing HZSM-5-X carrier by hydrothermal synthesis, wherein the specific surface area reaches 320-417m2/g。
Finally, La (NO) is impregnated by the impregnation method3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2Impregnating O in HZSM-5-X carrier, controlling the molar ratio of La to Mn to W to be 1:1:0.2-0.25, and preparing W-LaMnO by temperature programming and calcining3The catalyst is/HZSM-5-X catalyst.
W-LaMnO prepared in example 1 above3Catalyst of/HZSM-5-X (X50, 100,150,200,250,300) in valeraldehyde (C)5H10O) concentration of 210ppm under the condition of air at 200 ℃, the catalytic efficiency is 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-LaMnO3HZSM-5-100. As the reaction proceeds, the catalytic efficiency proceeds with SiO2/Al2O3The proportion is increased first and then decreased, except W-LaMnO3W-LaMnO outside HZSM-5-3003(ii) p-valeraldehyde (C) HZSM-5-X (50, 100,150,200,250,300 ═ X)5H10O) was higher than 96%, as shown in fig. 1, 2.
W-LaMnO prepared in example 13HZSM-5-X (X50, 100,150,200,250,300) catalyst at 2 vol.% H2W-LaMnO under O condition3HZSM-5-50 and W-LaMnO3HZSM-5-100 p-valeraldehyde (C)5H10O) to 100%. With SiO2/Al2O3Increase in the ratio H2The promotion effect of O on the catalytic efficiency is reduced, but the reduction range is within 5 percent, and the total catalytic efficiency is more than95 percent. As shown in fig. 3 and 4.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (7)
1. A preparation method of a multi-stage micro-mesoporous low-temperature catalyst is characterized in that the catalyst is represented by the following general formula (1),
W-LaMnO3/HZSM-5-X … general formula (1)
In the general formula (1), HZSM-5-X is a carrier, and X represents SiO2With Al2O3The ratio of the molar ratio, wherein X is 50-300; the molar ratio of W to La to Mn is (0.2-0.25) to 1: 1;
the method comprises the following steps:
extraction of SiO from fly ash2And Al2O3Extracting SiO2And Al2O3Proportionally with Na2Mixing O and tetrapropylammonium hydroxide step by step, stirring and heating to form gel;
mixing the gel and poly dimethyl diallyl ammonium chloride in proportion to prepare an HZSM-5-X carrier;
la (NO) by impregnation method3)3、Mn(NO3)2、3(NH4)2O-7WO3-6H2O is impregnated in the HZSM-5-X carrier, and the W-LaMnO is prepared by temperature programming and calcination3The catalyst is/HZSM-5-X catalyst.
2. The method of claim 1, wherein the extracting SiO from fly ash is performed2And Al2O3The method comprises the following steps:
calcining fly ash and NaOH, and extracting SiO by leaching method2And Al2O3。
3. The preparation method as claimed in claim 2, characterized in that the fly ash is calcined at a temperature of 750-850 ℃ for 2.2-2.6 hours and then mixed with NaOH at a temperature of 820-860 ℃ for 2.5-3.2 hours to obtain a calcined product; cooling the calcined product to 46-55 ℃, adding 3mol/L HCl to control the liquid-solid ratio to be 10:1, and stirring for 2.5-3.2 hours to obtain sol rich in Si and Al substances; adjusting the pH and introducing CO2Filtering, separating, washing and drying to obtain SiO2And Al2O3。
4. The method according to claim 1, wherein the molar ratio of each substance in the gel is H2O:SiO2:Al2O3:Na2O is tetrapropylammonium hydroxide (20: 100: X:0.12: 0.2), X is 100/X; x represents SiO2With Al2O3Ratio of molar ratio.
5. The preparation method according to claim 1, wherein the HZSM-5-X carrier is prepared by mixing the gel with poly (dimethyldiallylammonium chloride) in proportion and performing hydrothermal synthesis.
6. The process according to claim 5, wherein the HZSM-5-X support is usedSpecific surface area of 320-417m2/g。
7. The process according to claim 1, wherein the molar ratio of W to La to Mn is controlled to be (0.2-0.25) to 1, and LaMnO is controlled to be3Is 10% by weight.
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