CN115155580A - High-chlorine-resistance and thermal-aging-resistance catalyst for catalytic combustion of organic waste gas and preparation method thereof - Google Patents
High-chlorine-resistance and thermal-aging-resistance catalyst for catalytic combustion of organic waste gas and preparation method thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/656—Manganese, technetium or rhenium
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- B01J33/00—Protection of catalysts, e.g. by coating
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses a high chlorine resistance and thermal aging resistance catalyst for catalytic combustion of organic waste gas, which is characterized in that: the catalyst is a rare earth material with good chemical stability, chlorine resistance and sulfur resistance, which is covered on the surface of a manganese oxide supported noble metal catalyst; the problems of poor heat aging resistance and short service life of the catalyst are solved, the catalytic activity, the toxicity resistance and the heat aging resistance of the catalyst are improved, and the service life of the catalyst is prolonged.
Description
Technical Field
The invention relates to the field of organic waste gas treatment, in particular to a high-chlorine-resistance and heat-aging-resistance catalyst for catalytic combustion of organic waste gas and a preparation method thereof.
Background
Volatile Organic Compounds (VOCs) are important precursor substances for haze and ozone generation, and are directly discharged into the atmosphere to cause atmospheric pollution. VOCs have stronger toxicity, and particularly chlorine-containing VOCs have higher toxicity and larger degradation coefficient, thus being harmful to human health. Among the treatment technologies of the VOCs, the catalytic combustion technology is most widely applied, and the VOCs are catalytically decomposed into carbon dioxide and water by the aid of a catalyst, so that the treatment efficiency is relatively high. At present, there are many catalysts for catalytic combustion of industrial organic waste gas, and the catalysts are mainly divided into two categories. The catalytic activity of the noble metal catalyst is far higher than that of a non-noble metal catalyst, but the commercial application of the noble metal catalyst is limited by the defects of high price, easy agglomeration, easy poisoning, poor thermal aging resistance and the like, so that the dispersion degree of the noble metal catalyst needs to be improved by means of a carrier, and the effective utilization rate and the stability of the noble metal catalyst are improved. Although the catalytic activity of the non-noble metal catalyst is lower than that of a noble metal catalyst, the non-noble metal catalyst has various types, wide sources and low price, and particularly, the transition metal oxide can be used as the catalyst alone or as a carrier to generate a synergistic effect with other active components such as noble metals and the like, so that the catalytic activity of the catalyst is improved. Catalytic combustion of chlorine-containing VOCs requires higher reaction temperatures and higher selectivity. Although the Ru/OMS-2 catalyst can improve the effective utilization rate of Ru, reduce the cost and show excellent catalytic activity, the mixed valence state in the OMS-2 structure is easily influenced by temperature.
Disclosure of Invention
In view of the above, the present invention aims to provide a high chlorine resistance and thermal aging resistance catalyst for catalytic combustion of organic exhaust gas and a preparation method thereof, so as to solve the problems of poor thermal aging resistance and short service life of the catalyst, improve the catalytic activity, the poisoning resistance and the thermal aging resistance of the catalyst, and prolong the service life of the catalyst.
The catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic waste gas is prepared by covering a layer of rare earth material with good chemical stability, chlorine resistance and sulfur resistance on the surface of a manganese oxide supported noble metal catalyst;
furthermore, the catalyst is prepared by covering a layer of CeO on the surface of a Ru/OMS-2 catalyst 2 Prepared Ru/OMS-2@ CeO 2 ；
Further, the Ru/OMS-2 catalyst is prepared by an impregnation method;
further, the supported amount of Ru is 0.1-0.5% by weight based on the manganese oxide.
The preparation method of the catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic waste gas comprises the following steps:
a. preparing OMS-2 by a hydrothermal method;
b. preparing Ru/OMS-2 by an impregnation method;
c.Ru/OMS-2@CeO 2 adding terephthalic acid into an N, N-dimethylformamide solution, performing ultrasonic treatment until the terephthalic acid is completely dissolved, then adding a salt solution of Ce for ultrasonic dissolution, then dropwise adding glacial acetic acid, continuing ultrasonic treatment, performing hydrothermal crystallization, centrifugation and washing on the obtained transparent solution to obtain a white precipitate, then dispersing the white precipitate into an ethanol aqueous solution, adding Ru/OMS-2, performing ultrasonic treatment, and then placing on a magnetic stirrer for continuing stirring; through suction filtration, washing, drying, calcining or aging, ru/OMS-2@ CeO is obtained 2 A catalyst;
further, in the step a, slowly dripping a potassium permanganate aqueous solution into a manganese acetate aqueous solution under the condition of magnetic stirring at room temperature, heating for a period of time at a certain temperature, and filtering, washing, drying and calcining to obtain an OMS-2 manganese oxide octahedral molecular sieve sample;
further, in the step a, the mass ratio of the potassium permanganate to the manganese acetate is 2:1-5;
further, in step b, OMS-2 was dispersed in RuCl 3 Stirring and soaking the solution at room temperature for a period of time, and then filtering, washing, drying and calcining the solution to prepare Ru/OMS-2;
further, in step c, the salt solution of Ce is Ce (NO) 3 ) 3 ·6H 2 O, the volume ratio of ethanol to water in the ethanol aqueous solution is 1:1;
furthermore, in the step c, the calcining temperature is 450-550 ℃, and the aging temperature is 550-650 ℃.
The invention has the beneficial effects that: the high-chlorine-resistance and heat-aging-resistance catalyst for catalytic combustion of organic waste gas and the preparation method thereof solve the problems of poor heat-aging-resistance and short service life of the catalyst, improve the catalytic activity, the toxicity resistance and the heat-aging resistance of the catalyst and prolong the service life of the catalyst.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
The catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic waste gas is prepared by covering a layer of rare earth material with good chemical stability, chlorine resistance and sulfur resistance on the surface of a manganese oxide supported noble metal catalyst; the surface of the catalyst is coated with a layer of rare earth material with the characteristics of good chemical stability, chlorine resistance, sulfur resistance and the like, so that the chlorine poisoning resistance and the heat aging resistance of the catalyst are enhanced, the application range is enlarged, and the service life is prolonged.
In this example, the catalyst was prepared by coating a layer of CeO on the surface of a Ru/OMS-2 catalyst 2 Prepared Ru/OMS-2@ CeO 2 (ii) a The octahedral molecular sieve (OMS-2) is used as a manganese oxide, has the advantages of the molecular sieve and the manganese oxide, can be used as a catalyst to be used alone, and can also be used as a carrier to generate a synergistic effect with an active component. The organic waste gas can be adsorbed on the surface of the catalyst in a large amount and is fully contacted with the active component; under the condition of coexistence of multi-valence state manganese ions, the oxidation-reduction capability of the catalyst is improved, and the conversion of organic waste gas is accelerated; meanwhile, OMS-2 has mild surface acidity and alkalinity, and is beneficial to the breaking of bonds such as C-Cl, C-N and the like. The Ru/OMS-2 catalyst can improve the effective utilization rate of Ru, reduce the cost and show excellent catalytic activity. However, the mixed valence state in the OMS-2 structure is easily influenced by temperature, so that a layer of material with the characteristics of good chemical stability, excellent biocompatibility, chlorine resistance, sulfur resistance and the like is wrapped on the surface of the catalyst, the heat aging resistance of the catalyst is improved, and the catalytic activity of the catalyst is improved. CeO (CeO) 2 As an excellent catalyst auxiliary agent, the catalyst has good oxygen storage and release capacity and oxidation reduction capacity, and is beneficial to the catalytic combustion reaction. Using MOFs material as template, passing through highCalcining at a low temperature to make the organic ligand in the template to be CO 2 、H 2 And O (g) or other gas forms overflow from the template, so that a porous material can be formed, and meanwhile, metal ions or metal clusters are converted into metal oxides in a calcining atmosphere or metal atoms are attached to the surface of the porous material to form the nano-porous metal oxide.
And a layer of CeO is covered on the surface of the Ru/OMS-2 catalyst 2 The thermal aging resistance of the Ru/OMS-2 can be improved, the catalytic activity of the catalyst can be improved, and the catalyst has breakthrough significance for the development of catalytic combustion of chlorine-containing VOCs by using the manganese oxide-supported noble metal catalyst. Ru/OMS-2@ CeO for catalytic combustion of organic waste gas 2 The concentration of the catalyst at the inlet of a reaction substrate is 1100ppm, and the space velocity is 45000 mL-g -1 ·h -1 Under the conditions of (1, 2-dichloroethane) catalytically combusting 85 340 ℃, compared with a Ru/OMS-2 catalyst, the required reaction temperature is reduced by 20 ℃ under the same conversion rate, and the catalytic activity is high; meanwhile, the catalyst has good thermal aging resistance, the activity of catalyzing 1, 2-dichloroethane is greatly reduced after the Ru/OMS-2 catalyst is aged at 600 ℃, and CeO is added 2 The catalytic activity of the catalyst is basically kept unchanged after the catalyst is aged at 600 ℃.
In this example, the supported amount of Ru is 0.1 to 0.5% by weight, preferably 0.2% by weight, based on the manganese oxide.
The preparation method of the catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic waste gas of the embodiment comprises the following steps:
a. preparing OMS-2 by a hydrothermal method;
b. preparing Ru/OMS-2 by an impregnation method;
c.Ru/OMS-2@CeO 2 adding terephthalic acid into an N, N-dimethylformamide solution, performing ultrasonic treatment until the terephthalic acid is completely dissolved, then adding a salt solution of Ce for ultrasonic dissolution, then dropwise adding glacial acetic acid, continuing ultrasonic treatment, performing hydrothermal crystallization, centrifugation and washing on the obtained transparent solution to obtain a white precipitate, then dispersing the white precipitate into an ethanol aqueous solution, adding Ru/OMS-2, performing ultrasonic treatment, and then placing on a magnetic stirrer for continuing stirring; through filtering, washing, drying, calcining or aging, ru/OMS-2@CeO 2 A catalyst; the preparation method is simple and controllable.
In the embodiment, in the step a, a potassium permanganate aqueous solution is slowly dropped into a manganese acetate aqueous solution under the condition of magnetic stirring at room temperature, hydrothermal is carried out for a period of time at a certain temperature, and an OMS-2 manganese oxide octahedral molecular sieve sample is obtained after filtering, washing, drying and calcining; the mass ratio of the potassium permanganate to the manganese acetate is 2:1-5, preferably 2/3.
In this example, OMS-2 was dispersed in RuCl in step b 3 Stirring and dipping the solution for a period of time at room temperature, filtering, washing, drying and calcining to prepare Ru/OMS-2; in step c, the salt solution of Ce is Ce (NO) 3 ) 3 ·6H 2 O, the volume ratio of ethanol to water in the ethanol aqueous solution is 1:1; in step c, the calcination temperature is 450-550 ℃, the aging temperature is 550-650 ℃, ru/OMS-2@ CeO 2 The mass fraction in terms of Ru/OMS-2 in the preparation process is 0, 0.18, 0.22 and 0.30, preferably 0.18.
Example one
Preparation of OMS-2: respectively dissolving potassium permanganate and manganese acetate in distilled water to prepare solution, and under the condition of magnetic stirring at room temperature, adding 40mL of 0.175mol.L -1 Slowly dropping a potassium permanganate solution into 10mL of a manganese acetate solution, stirring for 2h, transferring the mixed solution into a 100mL stainless steel reaction kettle with polytetrafluoroethylene, and heating for 24h at 100 ℃; filtering, and washing with distilled water for several times; drying at 80 deg.C, placing in muffle furnace at a heating rate of 5 deg.C/min -1 Heating to a certain temperature and keeping for 4h under the condition of (1) to obtain tan OMS-2 powder.
Preparation of Ru/OMS-2: taking 8mL of RuCl with a certain concentration 3 Putting the solution into a beaker, and adding 12mL of distilled water for dilution; adding 0.5g of OMS-2 powder prepared in example 1, stirring and immersing at room temperature for 12h; and (3) completely drying in a drying oven, and calcining at 500 ℃ for 4h to obtain the Ru/OMS-2 catalyst.
Ru/OMS-2@CeO 2 The preparation of (1): 0.1250g of terephthalic acid (H) 2 BDC) was added to 40mL of N, N-Dimethylformamide (DMF) and sonicated to H 2 BDC is completely dissolved; 0.217gCe (N) was addedO 3 ) 3 ·6H 2 O, performing ultrasonic treatment for 10min; then 1.5mL of glacial acetic acid is added dropwise, and the ultrasonic treatment is continued for 10min; transferring the transparent solution into a reaction kettle, and carrying out hydrothermal crystallization at 120 ℃ for 28 hours; centrifuging and washing for several times; dispersing the obtained white precipitate into 60mL of ethanol water solution, adding 0.3g of the Ru/OMS-2 catalyst prepared in the example 2, carrying out ultrasonic treatment for 30min, and then placing on a magnetic stirrer to stir at room temperature for 6h; carrying out suction filtration and washing for a plurality of times; completely drying at 80 deg.C; roasting at 500 deg.C for 4h to obtain Ru/OMS-2@ CeO 2 A catalyst.
And (3) activity test:
1. Ru/OMS-2 catalyst Activity test: the catalytic combustion reaction of the organic waste gas is carried out on a fixed reaction bed reaction device with an online multi-dimensional gas chromatograph. Taking the mixed gas of 1, 2-dichloroethane and air as inlet air, passing through Ru/OMS-2@ CeO 2 The catalyst reacts, and the total flow of the mixed gas is controlled to be 99 mL/min by a flowmeter -1 The concentration of 1, 2-dichloroethane was controlled to 1100ppm by flow regulation, and the space velocity of the reaction was 45000mL · g -1 ·h -1 The reaction temperature is 300-400 ℃, the reaction is stable for 20-30 min every 20 ℃, gas components before and after the reaction are analyzed on line by Japan Shimadzu GC-2014 multidimensional gas chromatography, and the conversion rate reaches 85% at the temperature of 360 ℃.
2、Ru/OMS-2@CeO 2 And (3) testing the activity of the catalyst: the test conditions are the same as above, and the test result is as follows: the conversion rate of 1, 2-dichloroethane reaches 99% at a temperature of 360 ℃.
Example two
Respectively placing the fresh catalysts prepared in the first embodiment at 600 ℃ for heat aging for 4h; the method is not in a calcining mode, is in an aging treatment mode, and has the same steps as the first embodiment.
And (3) activity test: the activity was tested under the same conditions as in example one, at a temperature of 360 ℃ with a conversion of 1, 2-dichloroethane of 99%.
Comparative example 1
The Ru/OMS-2 catalyst obtained in example I (dried fresh catalyst) was heat-aged at 600 ℃ for 4h. (direct heat aging treatment after drying, without calcination treatment)
And (3) activity test: the activity was tested under the same conditions as in example one, at a temperature of 360 ℃ and a conversion of 1, 2-dichloroethane of 65%.
Comparative example 2
0.2170g Ce (NO) 3 ) 3 ·6H 2 Adding O into a round-bottom flask, and dissolving with 10mL of distilled water; controlling the speed by using a constant-pressure funnel, and gradually dripping 100mL of ethanol aqueous solution containing 0.2103g of hexamethylenetetramine; refluxing at 60 deg.C for 2 hr to obtain white precipitate, stopping heating, and cooling to room temperature; adding 0.3g of Ru/OMS-2 catalyst, and stirring at room temperature for 6 hours; carrying out suction filtration and washing for a plurality of times; completely drying at 80 deg.C; roasting at 500 deg.C for 4h to obtain Ru/OMS-2@ CeO prepared by chemical precipitation 2 A catalyst.
And (3) activity test: the activity was tested under the same conditions as in example one, at a temperature of 360 ℃ and a conversion of 1, 2-dichloroethane of 70%.
EXAMPLE III
Preparation of OMS-2: respectively dissolving potassium permanganate and manganese acetate in distilled water to prepare a solution, slowly dripping the potassium permanganate solution into the manganese acetate solution under the state of magnetic stirring at room temperature, then stirring for 2.5 hours, transferring the mixed solution into a 100mL stainless steel reaction kettle with polytetrafluoroethylene, and heating for 24 hours at 100 ℃; filtering, and washing with distilled water for several times; after being completely dried at 85 ℃, the mixture is placed in a muffle furnace at the temperature rise rate of 5 ℃ min -1 Heating to a certain temperature and keeping for 4h under the condition of (1) to obtain brown OMS-2 powder. The mass ratio of the potassium permanganate to the manganese acetate is 2:1-5.
Preparation of Ru/OMS-2: taking RuCl 3 Putting the solution in a beaker, and adding distilled water for dilution; adding OMS-2 powder, stirring at room temperature, and soaking for 14h; and (3) completely drying in a drying oven, and calcining at 450 ℃ for 4h to obtain the Ru/OMS-2 catalyst. The loading of Ru was 0% by weight based on manganese oxide.
Ru/OMS-2@CeO 2 The preparation of (1): 0.1250g of terephthalic acid (H) 2 BDC) was added to 40mL of N, N-Dimethylformamide (DMF) and sonicated to H 2 BDC is completely dissolved; 0.217gCe (NO) was added 3 ) 3 ·6H 2 O, performing ultrasonic treatment for 10min; then 1.5mL of glacial acetic acid is added dropwise, and the ultrasonic treatment is continued for 10min; transferring the transparent solution into a reaction kettle,hydrothermal crystallization at 120 ℃ for 28h; centrifuging and washing for several times; dispersing the obtained white precipitate in 60mL of ethanol water solution, adding 0.3gRu/OMS-2 catalyst, performing ultrasonic treatment for 30min, and stirring for 6h at room temperature on a magnetic stirrer; carrying out suction filtration and washing for several times; completely drying at 80 deg.C; roasting at 550 deg.C for 4h to obtain Ru/OMS-2@ CeO 2 A catalyst.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic waste gas is characterized in that: the catalyst is a rare earth material with good chemical stability, chlorine resistance and sulfur resistance, which is covered on the surface of a manganese oxide supported noble metal catalyst.
2. The catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 1, characterized in that: the catalyst is prepared by covering a layer of CeO on the surface of a Ru/OMS-2 catalyst 2 Prepared Ru/OMS-2@ CeO 2 。
3. The catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 2, characterized in that: the Ru/OMS-2 catalyst was prepared by an impregnation method.
4. The catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 3, wherein: the loading amount of Ru is 0.1-0.5% by weight of manganese oxide.
5. The method for preparing a catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 1, wherein: the method comprises the following steps:
a. preparing OMS-2 by a hydrothermal method;
b. preparing Ru/OMS-2 by an impregnation method;
c.Ru/OMS-2@CeO 2 adding terephthalic acid into N, N-dimethylformamide solution, performing ultrasonic treatment until the terephthalic acid is completely dissolved, then adding Ce salt solution, performing ultrasonic dissolution, then dropwise adding glacial acetic acid, performing continuous ultrasonic treatment, performing hydrothermal crystallization, centrifugation and washing on the obtained transparent solution to obtain white precipitate, then dispersing the white precipitate into ethanol water solution, adding Ru/OMS-2, performing ultrasonic treatment, and then placing on a magnetic stirrer for continuous stirring; through suction filtration, washing, drying, calcining or aging, ru/OMS-2@ CeO is obtained 2 A catalyst.
6. The method for preparing a catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 5, wherein: in the step a, slowly dripping potassium permanganate aqueous solution into manganese acetate aqueous solution under the condition of room temperature magnetic stirring, heating for a period of time at a certain temperature, and filtering, washing, drying and calcining to obtain an OMS-2 manganese oxide octahedral molecular sieve sample.
7. The method for preparing the catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 6, wherein: in the step a, the mass ratio of the potassium permanganate to the manganese acetate is 2:1-5.
8. The method for preparing a catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 7, wherein: in step b, OMS-2 is dispersed in RuCl 3 And stirring and soaking the solution at room temperature for a period of time, and then filtering, washing, drying and calcining the solution to obtain the Ru/OMS-2.
9. The high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 8The preparation method of the catalyst is characterized in that: in step c, the salt solution of Ce is Ce (NO) 3 ) 3 ·6H 2 O, the volume ratio of ethanol to water in the ethanol aqueous solution is 1:1.
10. the method for preparing a catalyst with high chlorine resistance and thermal aging resistance for catalytic combustion of organic exhaust gas according to claim 9, wherein: in the step c, the calcining temperature is 450-550 ℃, and the aging temperature is 550-650 ℃.
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