CN115400745A - Cerium-based catalyst for efficiently degrading CVOCs (chemical vapor deposition) - Google Patents
Cerium-based catalyst for efficiently degrading CVOCs (chemical vapor deposition) Download PDFInfo
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Abstract
The invention discloses a cerium-based catalyst for efficiently degrading CVOCs (chemical vapor deposition) and a preparation method thereof. M-V/CeO prepared by the process of the invention 2 The catalyst has good low-temperature activity, high conversion rate and high CO content 2 Selectivity, reduces the decomposition and oxidation temperature of the CVOCs, improves the chlorine poisoning resistance of the catalyst, and improves the performance of the catalyst, thereby being beneficial to the high-efficiency degradation of the CVOCs. In addition, the preparation process is simple and easy to operate, the used precious metal elements are few, and other metal elementsThe cost is low, the resource is rich, and the application prospect is wide.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a cerium-based catalyst for efficiently degrading CVOCs (chemical vapor deposition catalysts).
Background
Following particulate matter, sulfur dioxide, nitrogen oxides, volatile Organic Compounds (VOCs) have become part of the most common atmospheric pollutants. chlorine-Containing Volatile Organic Compounds (CVOCs) are pollutants with higher toxicity and more difficult treatment of Volatile Organic Compounds (VOCs), have the characteristics of high toxicity, high stability, difficult degradation and the like, and are widely generated in various fields of industry, agriculture, medicines, organic synthesis and the like. Researches show that CVOCs have great influence on ecological environment and human health, such as ozone layer damage, photochemical smog and the like, and human bodies are easy to accumulate in vivo after being contacted for a long time and have strong carcinogenicity.
According to the related reports, various CVOCs treatment technologies such as adsorption method, absorption method, low-temperature plasma method, photocatalytic oxidation method, biological treatment method, catalytic combustion method, etc. have been developed. The catalytic combustion method has been widely studied and applied due to the advantages of low initiation temperature, high treatment efficiency, no secondary pollution and the like. The core of the catalytic combustion method lies in the development of a catalyst, and a proper catalyst system is selected so as to efficiently degrade CVOCs waste gas. An ideal CVOCs catalyst should have the advantages of low cost, high activity, high stability and durability. Generally, a common catalyst system is a noble metal, transition metal oxide catalyst, depending on the catalyst active component. Noble metal catalysts generally exhibit excellent activity in CVOCs catalytic oxidation reactions, but are expensive and have poor resistance to chlorine poisoning, particularly in the treatment of chlorine-containing organic exhaust gases, and are susceptible to catalyst deactivation by poisoning. Although the oxidation activity of the transition metal catalyst is not high, the transition metal catalyst has low price, various combination modes and strong chlorine poisoning resistance, and is an ideal substitute of a noble metal catalyst. Compared with the single-metal catalyst, the catalyst has the advantages that,the bimetallic catalyst can utilize the advantages of synergy and electronic effect among metals, improve the disadvantages of the single metal catalyst, reduce the consumption of noble metals, reduce the cost of the catalyst and improve the performance of the catalyst. In which CeO is present 2 Is a rare earth metal oxide, has unique redox characteristics, abundant oxygen vacancies and low cost, and is of great interest. However, ceO in a single component 2 When the catalyst is used for catalyzing and burning CVOCs, the active center of the catalyst is covered and the deactivation phenomenon occurs due to the strong adsorption of chlorine species on the active center. Therefore, a highly active, ceO compound has been developed 2 There is a need for cerium-based catalysts that have good interaction with other components while having strong resistance to chlorine poisoning.
CN101444746B patent discloses a CeO 2 The preparation method of the molecular sieve catalyst takes cerous nitrate and a molecular sieve with strong acidity as raw materials and adopts a mechanical grinding method to prepare CeO 2 -a molecular sieve catalyst. The preparation process is simple, low in cost and high in catalytic degradation activity on chlorine-containing organic compounds such as dichloromethane, dichloroethane and trichloroethylene. However, single component of CeO 2 When the catalyst is used for catalyzing and burning VOCs, the deactivation phenomenon is easy to occur, and the chlorine poisoning resistance is poor. In addition, prepared by milling, ceO 2 The catalyst is unevenly distributed on the surface of the molecular sieve, so that the catalytic activity of the catalyst is reduced.
CN101829568A discloses a preparation method and application of a manganese oxide in-situ doped palladium-based monolithic catalyst. The preparation method comprises the steps of coprecipitating a manganese oxide precursor and metal palladium on the surface of honeycomb ceramics, and roasting at high temperature to obtain the manganese oxide species in-situ doped palladium-based monolithic catalyst. At airspeed of 10000h -1 Toluene concentration of 4g/m 3 Under the condition of (2), the catalyst can ensure that the conversion rate of toluene reaches more than 90 percent at a lower temperature (215-228 ℃). However, for the spraying industry and the pharmaceutical industry, the VOC exhaust gas usually has the characteristics of high concentration and high space velocity, and the cost of the noble metal is high, so the VOC exhaust gas has certain limitations in practical application, and is not suitable for large-scale industrial application.
The patent CN107308983B discloses a catalyst for removing indoor VOC at room temperature and a preparation method thereof. The catalyst carrier is a titanium-silicon molecular sieve TS-1 with a multi-stage pore channel, and the active component is a noble metal silicon dioxide composite material with a core-shell structure. At a VOC concentration of 100ppm, a reaction temperature of 30 ℃ and a gas volume space velocity of 400min -1 Under the condition, the VOC removal rate of the catalyst is about 82%, and the catalyst has strong adsorption capacity on different organic matters in the air and good water resistance. But the application range is small, the method is only suitable for catalytic oxidation removal of VOC in the air at room temperature, and VOC waste gas mainly comes from industrial production and cannot be applied to actual industry.
The CN109201077A patent discloses a catalyst for degrading VOCS waste gas in pharmaceutical industry and a preparation method thereof. The catalyst consists of an active component and a carrier, wherein the active component is a mixture of families IB, IIB, VIIB and VIII, and the carrier is modified diatomite. The catalyst has high reaction activity, good selectivity, low operation cost and less secondary pollutants. However, the catalyst has a difference from the noble metal catalyst in catalytic efficiency, and the catalyst is complex to prepare and difficult to apply in actual industry.
Currently, catalytic combustion is still a viable approach for treating CVOCs exhaust gas, but higher temperatures are generally required in catalytic combustion treatment, energy consumption increases with increasing combustion temperature, and economic cost for treating pollution gas is higher. In order to expand the application range and popularize the practical application, the use of expensive noble metals needs to be reduced, and on the premise of economy, the invention develops the cerium-based catalyst for efficiently degrading the CVOCs.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above problems and/or problems occurring in the prior art.
Accordingly, it is an object of the present invention to overcome the deficiencies of the prior art and to provide a cerium based catalyst for the efficient degradation of CVOCs.
In order to solve the technical problems, the invention provides the following technical scheme: a cerium-based catalyst for efficiently degrading CVOCs is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
the catalyst is a supported multi-element metal oxide catalyst and consists of active components and a carrier, wherein the active components comprise a first base metal element vanadium and a second metal element M, the second metal element M can be any one of Ru, cu, co and Mn, and the carrier is polycrystalline nano cerium oxide CeO 2 。
As a preferable embodiment of the cerium-based catalyst of the present invention, wherein: the precursor of the bulk polycrystalline nano cerium oxide is cerium nitrate hexahydrate (99.5%),
weighing 10 parts of Ce (NO) 3 ) 3 ·6H 2 Dissolving O acid salt in 80 parts of deionized water, performing ultrasonic oscillation to dissolve the O acid salt until no particles exist, adding 3 parts of urea to prepare a mixed solution, and violently stirring the mixed solution for 0.5 hour at room temperature by using a magnetic stirrer;
transferring the uniformly stirred mixed solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into a vacuum drying oven, crystallizing for 4-7 hours at the temperature of 120-160 ℃, and opening after cooling to room temperature;
and taking out the sample, filtering and washing the sample by using deionized water until the sample is neutral, washing the sample by using absolute ethyl alcohol for 3 times, drying the sample, and then putting the dried sample into a muffle furnace for roasting.
As a preferable embodiment of the cerium-based catalyst of the present invention, wherein: the precursor of the first base metal element vanadium is ammonium metavanadate (AR, 99%), and the loading capacity is 2%; the second metal element M is one of Ru, cu, co and Mn, the precursors are ruthenium trichloride (the pure Ru content is 45-55%), copper nitrate hexahydrate (AR, 99.0-102.0%), cobalt nitrate hexahydrate (AR, more than or equal to 98.5%) and manganese nitrate solution (50 wt%), the loading amount of Ru is 0.5%, and the loading amounts of Cu, co and Mn are all 3%.
As a preferable embodiment of the cerium-based catalyst of the present invention, wherein: the preparation process of the supported catalyst comprises the steps of dissolving active component precursors in different proportions in deionized water to form a metal salt solution with a certain concentration (if the loading capacity of the active component is x%, the mass ratio of the transition metal oxide to the cerium oxide is x (100-x)), and dissolving the active component precursors completely to form a dipping solution at room temperature by ultrasonic oscillation until no particles exist;
the prepared impregnation solution is used for impregnating the polycrystalline nano cerium oxide carrier, the impregnation process adopts a one-step method (single metal loading) or a multi-step method (multi-metal loading, and a sequential and respective loading mode) to carry out isometric impregnation, and the impregnation time is 12-18 h;
and drying the impregnated sample, and then putting the dried sample into a muffle furnace for roasting.
As a preferable embodiment of the cerium-based catalyst of the present invention, wherein: in the preparation process of the catalyst, the drying temperature is 80-100 ℃, and the drying time is 8-12 hours; the roasting temperature is 400-500 ℃, and the roasting time is 3-5 h.
As a preferable embodiment of the cerium-based catalyst of the present invention, wherein: the catalyst is tabletted and sieved, and then a sample with the particle size of 40-60 meshes is obtained.
As a preferable embodiment of the cerium-based catalyst of the present invention, wherein: the catalyst obtained by the preparation method is applied to catalytic combustion of chlorine-containing volatile organic pollutants.
As a preferable embodiment of the cerium-based catalyst of the present invention, wherein: in the catalytic combustion process, the concentration of the chlorine-containing volatile organic pollutants is 1000-2000 ppm, and the reaction space velocity is 20000-30000 mL/(g.h).
The invention has the beneficial effects that:
(1) M-V/CeO prepared by the process of the invention 2 The catalyst has good low-temperature activity, high conversion rate and high CO content 2 Selectivity, reduces the decomposition and oxidation temperature of the CVOCs, improves the chlorine poisoning resistance of the catalyst, and improves the performance of the catalyst, thereby being beneficial to the high-efficiency degradation of the CVOCs.
(2) The preparation method has the advantages of simple preparation process, easy operation, less amount of used noble metal elements, lower cost of other metal elements, rich resources and contribution to large-scale use.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced 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 based on these drawings without inventive exercise. Wherein:
FIG. 1 is a schematic view of a packed tube of a catalytic oxidation CVOCs catalyst of the present invention.
FIG. 2 shows the V/CeO loading in different amounts in examples 1 to 3 of the present invention 2 CVOCs catalytic oxidation performance test chart of catalyst.
FIG. 3 shows Ru-V/CeO with different active components in examples 1-3 of the present invention 2 CVOCs catalytic oxidation performance test chart of catalyst.
FIG. 4 shows M-V/CeO in examples 1 to 3 of the present invention 2 Morphology of polycrystalline nanocatalyst.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein, and it will be appreciated by those skilled in the art that the present invention may be practiced without departing from the spirit and scope of the present invention and that the present invention is not limited by the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Catalyst carrier CeO in the present example 2 The preparation method sequentially comprises the following steps: weighing a certain amount of cerous nitrate hexahydrate, dissolving in deionized water, dissolving by ultrasonic oscillation, adding a proper amount of urea under a magnetic stirrer, and continuously stirring for 0.5h. And transferring the uniformly stirred mixed solution into a high-pressure reaction kettle, crystallizing for 5 hours at the temperature of 140 ℃, and opening after cooling to room temperature. Finally, taking out the sample, washing the sample to be neutral by using deionized water and absolute ethyl alcohol, drying the sample, and then putting the dried sample into a muffle furnace to be roasted to obtain a carrier CeO 2 . Tabletting, pulverizing, sieving, and making into 40-60 mesh granule. Pure CeO 2 The CVOCs catalytic oxidation performance of the catalyst was tested as shown in fig. 2.
Example 2
In this example, V/CeO 2 The preparation method sequentially comprises the following steps: by NH 4 VO 3 Preparing a metal salt solution with a certain concentration as a precursor, and soaking the metal salt solution in a carrier CeO in an equal volume 2 In the impregnation process, one-step impregnation is adopted, and finally drying and roasting are carried out to obtain the supported V/CeO 2 A catalyst. The loading amounts of the transition metal vanadium in the catalyst were changed to 0.8%, 1.6%, 2.0%, 3.0%, 4.8%, and 8.0%, respectively. V/CeO with different loading amounts 2 The CVOCs catalytic oxidation performance of the catalyst was tested as shown in fig. 2. As can be seen from FIG. 2, V/CeO increases with VOx 2 The activity of the catalyst shows a tendency to increase first and then decrease. The results show that the activity of the catalyst can be obviously improved by adding a certain amount of VOx (the loading is less than 5 percent), and the conversion rate curve is obviously shifted to the low temperature direction. Especially when the loading amount of V is 2 percent, V/CeO 2 The activity of the catalyst is highest, therefore, M-V/CeO 2 The loading of V in the catalyst is most suitably 2%.
Example 3
In this example, M-V/CeO 2 The preparation method of the catalyst sequentially comprises the following steps: impregnating the polycrystalline nano cerium oxide carrier with a metal salt solution with a certain concentration by adopting a multi-step method in the impregnation process, and finally drying and roasting to obtain supported Ru-V/CeO 2 A catalyst. In which V isThe loading was 2% and the loading of Ru was 0.5%. M-V/CeO of different active components 2 The CVOCs catalytic oxidation performance of the catalyst was tested as shown in fig. 3. As can be seen from FIG. 3, concurrent loading of RuO 2 And V 2 O 5 Ru-V/CeO of 2 The catalytic activity of the catalyst is obviously improved.
M-V/CeO 2 Test of catalytic performance of catalyst degradation CVOCs
The invention is carried out on a fixed bed. The catalytic oxidation of methylene chloride was investigated using a glass quartz tube having an inner diameter of 6mm as a catalyst reactor. After grinding, tabletting and screening the used catalyst, 200mg of a sample with the particle size of 40-60 meshes is weighed and placed in a quartz tube reactor. Gas flow rate was controlled by mass flow meter, total flow rate was 100mL/min, reaction gas was measured by 1000ppm DCM, 20% 2 And N 2 The gas space velocity GHSV is 30000 mL/(g.h). Feeding liquid dichloromethane into vaporizing chamber by micro-sampling pump, mixing with O 2 And N 2 Mixing produces gaseous methylene chloride. The injection section was heated electrically to 80 ℃ to ensure complete evaporation of the liquid dichloromethane. The whole reaction pipeline is wrapped by a heating belt and heated to a temperature above the boiling point of the reaction gas to maintain stability so as to ensure that the reaction substrate exists in the reaction pipeline in a gaseous state. Before the test, reaction gas is continuously introduced for a period of time, so that the catalyst reaches an adsorption saturation state to eliminate concentration reduction caused by CVOCs adsorption. In the test process, reaction tail gas is monitored on line by adopting a gas chromatograph GC9790II, an ECD detector mainly analyzes chlorine-containing gas (dichloromethane and chlorine-containing byproducts), and an FID detector mainly analyzes CO and CO 2 。
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and 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 on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (8)
1. A cerium-based catalyst for efficiently degrading CVOCs is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
the catalyst is a supported multi-element metal oxide catalyst and consists of active components and a carrier, wherein the active components are a first base metal element vanadium and a second metal element M, the second metal element M can be any one of Ru, cu, co and Mn, and the carrier is polycrystalline nano cerium oxide CeO 2 。
2. The cerium-based catalyst for high-efficiency degradation of CVOCs according to claim 1, wherein: comprises that the precursor of the carrier polycrystal nanometer cerium oxide is cerium nitrate hexahydrate with the purity of 99.5 percent, and 10 parts of Ce (NO) are weighed 3 ) 3 ·6H 2 Dissolving O acid salt in 80 parts of deionized water, dissolving the O acid salt in the deionized water by ultrasonic oscillation until no particles exist, adding 3 parts of urea to prepare a mixed solution, and violently stirring the mixed solution for 0.5 hour at room temperature by using a magnetic stirrer;
transferring the uniformly stirred mixed solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into a vacuum drying oven, crystallizing for 4-7 hours at the temperature of 120-160 ℃, and opening after cooling to room temperature;
and taking out the sample, filtering and washing the sample by using deionized water until the sample is neutral, washing the sample by using absolute ethyl alcohol for 3 times, drying the sample, and then putting the dried sample into a muffle furnace for roasting.
3. The cerium-based catalyst for high-efficiency degradation of CVOCs as claimed in claim 1, wherein: the method comprises the following steps that a precursor of vanadium of a first base metal element is ammonium metavanadate, and the loading capacity is 2%; the second metal element M is one of Ru, cu, co and Mn, the precursors are ruthenium trichloride, copper nitrate hexahydrate, cobalt nitrate hexahydrate and a manganese nitrate solution respectively, wherein ammonium metavanadate is AR, the purity is 99%, the Ru content in the ruthenium trichloride is 45-55%, the copper nitrate hexahydrate is AR, the purity is 99.0%, the cobalt nitrate hexahydrate is AR, the purity is more than or equal to 98.5%, the mass fraction of the manganese nitrate solution is 50%, the loading capacity of Ru is 0.5%, and the loading capacities of Cu, co and Mn are 3%.
4. The cerium-based catalyst for high-efficiency degradation of CVOCs as claimed in claim 1, wherein: the preparation method comprises the steps of dissolving active component precursors in different proportions in deionized water to form a metal salt solution with a certain concentration, wherein if the loading capacity of the active components is x%, the mass ratio of the transition metal oxide to the cerium oxide is x (100-x), and the transition metal oxide and the cerium oxide are dissolved completely by ultrasonic oscillation at room temperature until no particles exist, so that an impregnation solution is formed;
impregnating the polycrystalline nano cerium oxide carrier by using the prepared impregnation solution, wherein the impregnation process adopts a one-step method, namely single metal loading or a multi-step method, namely multi-metal loading, and adopts a successively respective loading mode; carrying out equal-volume impregnation for 12-18 h;
and drying the impregnated sample, and then putting the dried sample into a muffle furnace for roasting.
5. The cerium-based catalyst for high-efficiency degradation of CVOCs as claimed in any one of claims 2 or 4, wherein: in the preparation process of the catalyst, the drying temperature is 80-100 ℃, and the drying time is 8-12 hours; the roasting temperature is 400-500 ℃, and the roasting time is 3-5 h.
6. The cerium-based catalyst for high-efficiency degradation of CVOCs as claimed in any one of claims 2 or 4, wherein: the catalyst is tabletted and sieved, and then a sample with the particle size of 40-60 meshes is obtained.
7. The cerium-based catalyst for high-efficiency degradation of CVOCs as claimed in claim 1, wherein: the catalyst obtained by the preparation method is applied to catalytic combustion of chlorine-containing volatile organic pollutants.
8. The cerium-based catalyst for high-efficiency degradation of CVOCs according to claim 1, wherein: in the catalytic combustion process, the concentration of the chlorine-containing volatile organic pollutants is 1000-2000 ppm, and the reaction space velocity is 20000-30000 mL/(g.h).
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2022
- 2022-07-28 CN CN202210896392.9A patent/CN115400745A/en active Pending
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| US5851948A (en) * | 1996-08-20 | 1998-12-22 | Hydrocarbon Technologies, Inc. | Supported catalyst and process for catalytic oxidation of volatile organic compounds |
| CN107051424A (en) * | 2017-03-22 | 2017-08-18 | 华东理工大学 | It is a kind of for catalyst of chlorinated hydrocarbon low-temperature catalytic burning and its preparation method and application |
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