CN115155579A - Reductive noble metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas and preparation method thereof - Google Patents
Reductive noble metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas and preparation method thereof Download PDFInfo
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- 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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- 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 reducing noble metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas, which is a manganese oxide loaded noble metal catalyst formed by dispersing noble metal on the surface of manganese oxide in a simple substance form, wherein a transition metal oxide which can be used as a catalyst and a carrier and a noble metal active component are adopted to generate a synergistic effect, so that the catalytic activity of the catalyst is improved, and a large amount of organic waste gas can be adsorbed on the surface of the catalyst 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. And the catalyst does not contain Cl, so that the problem of low utilization rate of the noble metal caused by the accumulation of byproducts formed by the reaction of the noble metal and the Cl on the surface of the carrier is avoided.
Description
Technical Field
The invention relates to the field of organic waste gas treatment, in particular to a reducing noble metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas and a preparation method thereof.
Background
Volatile Organic Compounds (VOCs) are important precursors 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. The industrial organic waste gas has various components, and the excellent catalyst for treating a single component is difficult to meet the actual requirement. 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 the 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 synergistic effect with other active components such as noble metals and the like, so that the catalytic activity of the catalyst is improved. The noble metal catalyst reported in the prior art mainly takes noble metals of Pt, pd and Ru as active components, and is loaded on metal oxide by means of impregnation and the like. The noble metal is easy to react with Cl species and the like to form byproducts, so that the byproducts are accumulated on the surface of the carrier, the utilization rate of the noble metal is low, and the wider application of the noble metal is limited.
Disclosure of Invention
In view of the above, the present invention aims to provide a reducing precious metal supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas and a preparation method thereof, which solve the problems that the existing precious metal catalyst is high in cost and easy to poison, and an impregnation process is easy to cause poor durability of active component surface aggregation.
The reducing noble metal-loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas is a manganese oxide-loaded noble metal catalyst formed by dispersing noble metals on the surface of manganese oxide in a simple substance form;
further, noble metal in the noble metal salt is dispersed on the surface of the manganese oxide in a simple substance form by adopting a chemical reduction method to form a manganese oxide supported noble metal catalyst;
further, the manganese oxide is OMS-2 and Mn 2 O 3 、Mn 3 O 4 MnO or the like;
further, the noble metal salt is one of platinum chloride, palladium chloride and ruthenium chloride solution;
furthermore, the loading amount of the noble metal is 0.1 to 0.5 percent by weight calculated by manganese oxide;
further, the noble metal salt is ruthenium chloride, the manganese oxide is OMS-2, and a ruthenium simple substance in the ruthenium chloride is dispersed on the surface of the OMS-2 by adopting a chemical reduction method to form the Ru/OMS-2 catalyst without Cl elements.
The invention discloses a preparation method of a reductive precious metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas, which is characterized by comprising the following steps: the method comprises the following steps:
a. preparing manganese oxide by a hydrothermal method;
b. preparing a manganese oxide supported noble metal catalyst: dispersing manganese oxide in deionized water, adding noble metal salt solution, adding reductant while stirring, centrifugal separation, washing with distilled water, and AgNO treatment 3 Detecting the filtrate by using the solution until no Cl ions are contained, and finally drying and calcining to obtain a Cl-element-free manganese oxide supported noble metal catalyst;
further, in step a, preparation of manganese oxide: respectively dissolving potassium permanganate and manganese acetate in deionized water, slowly dripping the potassium permanganate solution into the manganese acetate 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 manganese oxide;
further, in the step a, the mass ratio of potassium permanganate to manganese acetate is one of 2/1, 2/2, 2/3, 2/4 and 2/5;
further, the calcining temperature is 300-600 ℃, and in the step b, the reducing agent is sodium borohydride.
The invention has the beneficial effects that: according to the reductive precious metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic waste gas, the transition metal oxide which can be used as the catalyst and also as the carrier and the precious metal active component generate synergistic effect, so that the catalytic activity of the catalyst is improved, and a large amount of organic waste gas can be adsorbed on the surface of the catalyst and fully contacts 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. And the catalyst does not contain Cl, so that the problem of low utilization rate of the noble metal caused by the accumulation of byproducts formed by the reaction of the noble metal and Cl on the surface of the carrier is solved, the accumulation of Cl and the noble metal is effectively avoided compared with the traditional impregnation process, and the high efficiency of the catalyst is ensured. The manganese oxide supported noble metal catalyst prepared by the method is applied to 99000 mL/g -1 ·h -1 The space velocity of toluene organic waste gas is higher than the space velocity of 45000mL g -1 ·h -1 The catalytic activity of the organic waste gas containing 1, 2-dichloroethane at the space velocity is not much different from that of the catalyst containing Cl prepared by the traditional impregnation method, while the catalytic activity of the catalyst containing Cl is far better than that of the catalyst containing Cl prepared by the impregnation method, and the catalytic activity of the catalyst is far superior to that of the catalyst used in general commercial use.
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 reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas in the embodiment is a manganese oxide-supported noble metal catalyst formed by dispersing noble metals on the surface of manganese oxide in an elemental form; the noble metal is dispersed on the surface of the manganese oxide in a simple substance form, the transition metal oxide which can be used as a catalyst and a carrier is adopted to generate a synergistic effect with the active component of the noble metal, so that the catalytic activity of the catalyst is improved, and a large amount of organic waste gas can be adsorbed on the surface of the catalyst 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. And the catalyst does not contain Cl, so that the problem of low utilization rate of the noble metal caused by the accumulation of byproducts formed by the reaction of the noble metal and the Cl on the surface of the carrier is solved.
In the embodiment, noble metal in noble metal salt is dispersed on the surface of manganese oxide in a simple substance form by a chemical reduction method to form manganese oxide supported noble metal catalyst; a noble metal catalyst loaded with manganese oxide without Cl elements is prepared by adopting a chemical reduction method, and the catalyst is used for catalytic combustion of toluene and 1, 2-dichloroethane to obtain a multifunctional catalyst, thereby providing a new idea for treating VOCs with complex components.
In this embodiment, the manganese oxide is OMS-2, mn 2 O 3 、Mn 3 O 4 MnO or the like; OMS-2 is preferably used. The noble metal salt is one of platinum chloride, palladium chloride and ruthenium chloride solution;
in the embodiment, the loading amount of the noble metal is 0.1 to 0.5 percent by weight calculated by manganese oxide;
preferably, the noble metal salt is ruthenium chloride, the manganese oxide is OMS-2, and a chemical reduction method is adopted to disperse a ruthenium simple substance in the ruthenium chloride on the surface of the OMS-2 to form the Ru/OMS-2 catalyst without Cl elements. By chemical reduction of RuCl 3 Reducing the Ru into a simple substance which is highly dispersed on the surface of the catalyst. Compared with the traditional impregnation process, the method effectively avoids the accumulation of Cl species and noble metals, and ensures the high efficiency of the catalyst. Octahedral molecular sieve (OMS-2) as a manganese oxide with both molecular sieve and manganese oxideThe catalyst can be used alone as a catalyst, 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 preparation method of the reducing precious metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas comprises the following steps:
a. preparing manganese oxide by a hydrothermal method;
b. preparing a manganese oxide supported noble metal catalyst: dispersing manganese oxide in deionized water, adding noble metal salt solution, adding reductant under quick stirring, centrifugal separating, washing with distilled water, and adding AgNO 3 Detecting until the filtrate does not contain Cl ions by using a solution, and finally drying and calcining to obtain a Cl-element-free manganese oxide supported noble metal catalyst; the preparation method is simple.
In this example, in step a, preparation of manganese oxide: respectively dissolving potassium permanganate and manganese acetate in deionized water, slowly dripping the potassium permanganate solution into the manganese acetate solution under the state of magnetic stirring at room temperature, heating for a period of time at a certain temperature, and filtering, washing, drying and calcining to obtain manganese oxide; in the step a, the mass ratio of potassium permanganate to manganese acetate is one of 2/1, 2/2, 2/3, 2/4 and 2/5; the calcining temperature is 300-600 ℃, and in the step b, the reducing agent is sodium borohydride.
Example one
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 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; and (3) after completely drying at 80 ℃, putting the dried product in a muffle furnace, heating to a certain temperature under the condition that the heating rate is 5 ℃ min < -1 > and keeping for 4 hours to obtain an OMS-2 manganese oxide octahedral molecular sieve sample.
Ru/OMS-2 catalyst without Cl element: ruCl is added 3 The solution was placed in a beaker, diluted with distilled water, 0.5g OMS-2 was added and the appropriate amount of NaBH was added with stirring at room temperature 4 Stirring the solution for 12h, centrifuging, washing with distilled water for several times, and adding AgNO 3 Detecting until the filtrate does not contain Cl ions by using the solution, then completely drying at 80 ℃, and calcining for 4 hours at 300 ℃ to obtain the Ru/OMS-2 catalyst without Cl elements.
And (3) activity test:
1) Testing the activity of OMS-2 manganese oxide octahedral molecular sieve: the catalytic decomposition reaction of the organic waste gas is carried out on a fixed reaction bed reaction device with an online multi-dimensional gas chromatograph. When the mixed gas of 1, 2-dichloroethane and air is taken as inlet gas, the mixed gas is reacted by a Ru/OMS-2 catalyst, 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 control, and the reaction space velocity was 45000mL g -1 ·h -1 The reaction temperature is 300-400 ℃; when the mixed gas of toluene and air is taken as inlet gas, the mixed gas is reacted by Ru/OMS-2 catalyst, and the total flow of the mixed gas is controlled to be 165 mL/min by a flowmeter -1 The concentration of toluene was controlled to 1100ppm by flow control, and the space velocity of the reaction was 90000mL · g -1 ·h -1 The reaction temperature is 200-300 ℃. The reaction is stabilized at intervals of 20 ℃ for 20-30 min, and gas components before and after the reaction are analyzed on line by a multidimensional gas chromatography of Japan Shimadzu GC-2014. When the temperature of the catalyst is 340 ℃, the conversion rate of 1, 2-dichloroethane is 81 percent; at a temperature of 240 ℃, the toluene conversion was 82%.
2) The activity of the Ru/OMS-2 catalyst was tested: by adopting the method for testing the activity of the OMS-2 manganese oxide octahedral molecular sieve, the conversion rate of 1, 2-dichloroethane is 90% at the temperature of 340 ℃, and the conversion rate of toluene is 95% at the temperature of 240 ℃.
Comparative example 1:
using a common commercial catalyst carrier Al 2 O 3 Comparison with OMS-2:
and (3) activity test: the activity was tested under the same conditions as in example 1, except that the conversion of 1, 2-dichloroethane was 21% at a temperature of 340 ℃ and the conversion of toluene was 25% at a temperature of 240 ℃.
Comparative example 2
Preparation of Ru/Al without Cl element by chemical reduction method 2 O 3 The catalyst, the remaining steps were the same as for the Ru/OMS-2 catalyst of example one.
And (3) activity test: the activity was tested under the same conditions as in example 1, except that the conversion of 1, 2-dichloroethane was 62% at a temperature of 340 ℃ and the conversion of toluene was 68% at a temperature of 240 ℃.
Comparative example 3
The Ru/OMS-2 catalyst containing Cl element is prepared by an impregnation method. Taking RuCl with a certain concentration 3 Putting the solution into a beaker, and adding distilled water for dilution; adding 0.5g of OMS-2 prepared in example 1, stirring and immersing for 12h at room temperature; and (3) completely drying in a drying oven, and calcining at 300 ℃ for 4h to obtain the Ru/OMS-2 catalyst containing the Cl element.
And (3) activity test: the activity was tested under the same conditions as in example 1, except that the conversion of 1, 2-dichloroethane was 88% at a temperature of 340 ℃ and the conversion of toluene was 68% at a temperature of 240 ℃.
Example two
Preparation of manganese oxide Mn by conventional hydrothermal method 2 O 3 The platinum chloride solution is placed in a beaker, diluted by adding distilled water, then platinum chloride is added and a proper amount of NaBH is added under stirring at room temperature 4 Stirring the solution for 11h, centrifuging, washing with distilled water for several times, and AgNO 3 Detecting the filtrate with solution until no Cl ions are contained, completely drying at 75 ℃, calcining at 600 ℃ for 2h to obtain Ru/Mn without Cl elements 2 O 3 A catalyst. In this example, the supported amount of the noble metal was 0.1% by weight as the manganese oxide, and the amounts of the manganese oxide and platinum chloride added were calculated based on the supported amount. NaBH 4 Is added in an amount required to enable thorough reduction.
EXAMPLE III
Preparation of manganese oxide Mn by conventional hydrothermal method 3 O 4 The platinum chloride solution is put into a beaker and diluted by adding distilled waterThen palladium chloride is added and an appropriate amount of NaBH is added with stirring at room temperature 4 Stirring the solution for 13 hr, centrifuging, washing with distilled water for several times, and adding AgNO 3 Detecting the filtrate until no Cl ions are contained in the filtrate, completely drying at 85 ℃, and calcining at 400 ℃ for 3h to obtain Ru/Mn without Cl elements 2 O 3 A catalyst. In this example, the supported amount of the noble metal was 0.5% by weight as the manganese oxide, and the amounts of the manganese oxide and platinum chloride added were calculated based on the supported amount. NaBH 4 Is added in an amount required to enable thorough reduction.
Example four
Preparing manganese oxide MnO by adopting a conventional hydrothermal method, putting a platinum chloride solution into a beaker, adding distilled water for dilution, then adding palladium chloride, and adding a proper amount of NaBH under stirring at room temperature 4 Stirring the solution for 12h, centrifuging, washing with distilled water for several times, and adding AgNO 3 Detecting the filtrate until no Cl ions are contained in the filtrate, completely drying the filtrate at 80 ℃, and calcining the filtrate at 300 ℃ for 4 hours to obtain Ru/Mn without Cl elements 2 O 3 A catalyst. In this example, the supported amount of the noble metal was 0.3% by weight as the manganese oxide, and the amounts of the manganese oxide and platinum chloride added were calculated based on the supported amount. NaBH 4 Is added in an amount required to enable thorough reduction.
Finally, 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 various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A reducing noble metal loaded manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas is characterized in that: the catalyst is a manganese oxide supported noble metal catalyst formed by dispersing noble metal on the surface of manganese oxide in an elementary substance form.
2. The reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gases according to claim 1, characterized in that: noble metal in the noble metal salt is dispersed on the surface of the manganese oxide in a simple substance form by adopting a chemical reduction method to form the manganese oxide supported noble metal catalyst.
3. The reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gases according to claim 2, characterized in that: the manganese oxide is OMS-2 and Mn 2 O 3 、Mn 3 O 4 And MnO.
4. The reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gases according to claim 3, characterized in that: the noble metal salt is one of platinum chloride, palladium chloride and ruthenium chloride solution.
5. The reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gases according to claim 4, wherein: the loading amount of the noble metal is 0.1-0.5% by weight of manganese oxide.
6. The reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gases according to claim 5, characterized in that: the noble metal salt is ruthenium chloride, the manganese oxide is OMS-2, and a ruthenium simple substance in the ruthenium chloride is dispersed on the surface of the OMS-2 by adopting a chemical reduction method to form the Ru/OMS-2 catalyst without Cl elements.
7. The method for preparing a reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas according to claim 1, wherein: the method comprises the following steps:
a. preparing manganese oxide by a hydrothermal method;
b. preparing a manganese oxide supported noble metal catalyst:dispersing manganese oxide in deionized water, adding noble metal salt solution, adding reductant while stirring, centrifugal separation, washing with distilled water, and AgNO treatment 3 Detecting until the filtrate does not contain Cl ions by using a solution, and finally drying and calcining to obtain the Cl-element-free manganese oxide supported noble metal catalyst.
8. The method for preparing a reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas according to claim 7, wherein: in the step a, preparing manganese oxide: respectively dissolving potassium permanganate and manganese acetate in deionized water, slowly dripping the potassium permanganate solution into the manganese acetate solution under the state of magnetic stirring at room temperature, heating for a period of time at a certain temperature, and filtering, washing, drying and calcining to obtain the manganese oxide.
9. The method for preparing a reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas according to claim 8, wherein: in the step a, the mass ratio of potassium permanganate to manganese acetate is one of 2/1, 2/2, 2/3, 2/4 and 2/5.
10. The method for preparing a reducing noble metal-supported manganese oxide catalyst for catalytic combustion of multi-component organic exhaust gas according to claim 9, wherein: the calcining temperature is 300-600 ℃, and in the step b, the reducing agent is sodium borohydride.
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