CN112371106A - Synthesis method and application of Ce-Nb-O composite metal oxide catalyst - Google Patents
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Abstract
The invention discloses a synthesis method and application of a Ce-Nb-O composite metal oxide catalyst, wherein the synthesis method comprises the following steps: uniformly mixing deionized water, cerium nitrate, niobium oxalate and urea in a beaker according to a proportion, and then stirring and heating for reaction; and after the reaction is finished, naturally cooling, standing, performing suction filtration, and drying and calcining the obtained precipitate to obtain the Ce-Nb-O composite metal oxide catalyst. The raw materials adopted by the invention are cheap, the operation is simple and easy to repeat, and the obtained catalyst shows excellent catalytic degradation performance for several typical volatile organic pollutants.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a synthesis method and application of a Ce-Nb-O composite metal oxide catalyst.
Background
Volatile Organic Compounds (VOCs) refer to a class of Organic Compounds that are Volatile into the atmosphere at normal temperature and pressure, such as formaldehyde, ethanol, benzene, chlorobenzene, and the like. The organic matters are widely applied, are often used in the places of fine chemical synthesis, petrochemical industry, coal chemical industry, printing and dyeing, textile, packaging and transportation, home decoration and the like, and are substances with great harm in atmospheric pollutants.
For volatile organic pollutants, the most ideal solution is to reduce or even avoid the use of harmful substances. Under the condition that the use of the traditional Chinese medicine cannot be completely avoided, the thorough treatment is carried outIs particularly important. The post-treatment method of the volatile organic pollutants mainly comprises activated carbon adsorption, solvent absorption, low-temperature condensation, plasma/photocatalysis combination, high-temperature direct calcination and the like, and each method has respective application scenes and has advantages and disadvantages. In recent years, with the application and popularization of molecular sieve rotating wheel technology, the adsorption concentration/catalytic combustion method increasingly draws attention of people, has a good treatment effect on VOCs with low concentration, high wind speed, large capacity and complex components, and has the advantages of high treatment efficiency, low energy consumption, no secondary pollution and the like. The technical core of the catalytic combustion method is to develop a catalytic material with high catalytic activity, high stability and high selectivity. The traditional catalytic combustion method mainly aims at hydrocarbon and hydrocarbon oxygen pollutants, and commonly uses a supported noble metal catalyst (such as Pt/HZSM-5, Pt/CeO2/γ-Al2O3) The catalytic oxidation activity of (2) is high, but the price of noble metal is expensive, and if trace elements such as Cl, S, heavy metal and the like exist in the waste gas, the catalyst is easy to lose activity to cause the loss of treatment capability, so the catalyst is only applied in a part of occasions. In place of noble metal catalysts, base metal oxide catalysts have become the focus of current research, perovskites and CeO2-CrOx、V2O5-WO3/TiO2The catalyst system is representative. However, due to the problems of high preparation temperature of perovskite, small specific surface area of product and toxicity of Cr and V, the development of novel catalytic materials is urgently needed. In addition, due to the complexity of the components of industrial organic exhaust gases, a wide range of applications of the catalyst is also required, which can simultaneously eliminate various types of pollutants.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a synthesis method of a Ce-Nb-O composite metal oxide catalyst, and applies the method to the field of post-treatment of hydrocarbon and chlorohydrocarbon organic waste gases.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for synthesizing a Ce-Nb-O composite metal oxide catalyst comprises the following steps: uniformly mixing deionized water, cerium nitrate, niobium oxalate and urea in a beaker according to a proportion, and then stirring and heating for reaction; and after the reaction is finished, naturally cooling, standing, performing suction filtration, and drying and calcining the obtained precipitate to obtain the Ce-Nb-O composite metal oxide catalyst.
The dosage ratio of the metal elements in the niobium oxalate to the deionized water, the urea and the cerium nitrate is 0.1 mol: 50mL of: (4-22) mol: (0.1 to 1) mol.
The molar ratio of the sum of metal elements in the two raw materials of the cerium nitrate and the niobium oxalate to the urea is 1: 20.
the heating reaction temperature is 75-95 ℃, and the heating reaction time is 2-5 hours.
And naturally cooling the reacted mixture to room temperature, and then standing for 12-24 hours.
And the drying operation is to place the obtained precipitate in a drying oven and heat the precipitate to constant weight at the temperature of 90-120 ℃.
And the calcination operation is to place the dried powder in a muffle furnace for calcination for 2-5 hours at the temperature of 450-700 ℃.
The Ce-Nb-O composite metal oxide catalyst is prepared by compounding chemical elements Ce, Nb and O, wherein the molar ratio of the metal elements is Ce: nb (1-10): 1, and the balance of O element; the chemical composition of the Ce-Nb-O composite metal oxide catalyst can represent xCeO2-yNb2O5。
The application of the Ce-Nb-O composite metal oxide catalyst is used for catalytic combustion of several types of typical VOCs, and the catalyst shows excellent catalytic degradation performance.
Compared with the prior art, the invention has the beneficial effects that: (1) the raw materials used by the composite metal oxide catalyst are low in price and non-toxic, the high price of noble metals and the toxicity of Cr and V species in the traditional catalyst are avoided, and the synthesis steps are simple, safe and easy to repeat, so that the composite metal oxide catalyst is easy for large-scale production; (2) the catalyst synthesized by the method also has a long service life, and can resist high-temperature thermal shock of 700 ℃; (3) the composite metal oxide catalyst can fully play a role in the synergistic catalysis among elements Ce, Nb and O, has good catalytic deep oxidation promotion capability, has excellent catalytic combustion performance on a plurality of typical volatile organic pollutants, can be completely catalytically degraded at the reaction temperature of 300 ℃, and does not obviously reduce the catalytic activity in the process of continuous reaction for 168 hours.
Detailed Description
The invention is further described below with reference to specific embodiments:
synthesis of Ce-Nb-O composite metal oxide catalyst
Example 1: a method for synthesizing a Ce-Nb-O composite metal oxide catalyst comprises the following steps:
(1) adding 50mL of deionized water into a 250mL beaker, then adding a certain amount of cerous nitrate, niobium oxalate and urea, and stirring to uniformly mix the cerous nitrate, the niobium oxalate and the urea, wherein the dosage ratio of metal elements in the niobium oxalate to the deionized water, the urea and the cerous nitrate is 0.1 mol: 50mL of: 22mol of: 1mol to obtain a first mixture;
(2) reacting the first mixture in a beaker at the temperature of 80 ℃ for 5 hours, and then naturally cooling to room temperature to obtain a second mixture;
(3) standing the second mixture for 12 hours, then carrying out vacuum filtration, and heating the obtained precipitate in an oven at 120 ℃ to a constant weight state (removing water) to obtain a third mixture;
(4) and calcining the third mixture in a muffle furnace at the temperature of 450 ℃ for 5 hours, naturally cooling to room temperature, and grinding to obtain the Ce-Nb-O composite metal oxide catalyst which is marked as catalyst A.
Example 2: a method for synthesizing a Ce-Nb-O composite metal oxide catalyst comprises the following steps:
(1) adding 50mL of deionized water into a 250mL beaker, then adding a certain amount of cerous nitrate, niobium oxalate and urea, and stirring to uniformly mix the cerous nitrate, the niobium oxalate and the urea, wherein the dosage ratio of metal elements in the niobium oxalate to the deionized water, the urea and the cerous nitrate is 0.1 mol: 50mL of: 16mol of: 0.7mol to obtain a first mixture;
(2) reacting the first mixture in a beaker at 75 ℃ for 5 hours, and then naturally cooling to room temperature to obtain a second mixture;
(3) standing the second mixture for 18 hours, then carrying out vacuum filtration, and heating the obtained precipitate in an oven at 120 ℃ to a constant weight state (removing water) to obtain a third mixture;
(4) and calcining the third mixture in a muffle furnace at 500 ℃ for 4 hours, naturally cooling to room temperature, and grinding to obtain the Ce-Nb-O composite metal oxide catalyst which is marked as catalyst B.
Example 3: a method for synthesizing a Ce-Nb-O composite metal oxide catalyst comprises the following steps:
(1) adding 50mL of deionized water into a 250mL beaker, then adding a certain amount of cerous nitrate, niobium oxalate and urea, and stirring to uniformly mix the cerous nitrate, the niobium oxalate and the urea, wherein the dosage ratio of metal elements in the niobium oxalate to the deionized water, the urea and the cerous nitrate is 0.1 mol: 50mL of: 10 mol: 0.4mol to obtain a first mixture;
(2) reacting the first mixture in a beaker at 85 ℃ for 3 hours, and naturally cooling to room temperature to obtain a second mixture;
(3) standing the second mixture for 24 hours, then carrying out vacuum filtration, and heating the obtained precipitate in a 110 ℃ oven to a constant weight state (removing moisture) to obtain a third mixture;
(4) and calcining the third mixture in a muffle furnace at 550 ℃ for 4 hours, naturally cooling to room temperature, and grinding to obtain the Ce-Nb-O composite metal oxide catalyst which is marked as catalyst C.
Example 4: a method for synthesizing a Ce-Nb-O composite metal oxide catalyst comprises the following steps:
(1) adding 50mL of deionized water into a 250mL beaker, then adding a certain amount of cerous nitrate, niobium oxalate and urea, and stirring to uniformly mix the cerous nitrate, the niobium oxalate and the urea, wherein the dosage ratio of metal elements in the niobium oxalate to the deionized water, the urea and the cerous nitrate is 0.1 mol: 50mL of: 6 mol: 0.2mol to obtain a first mixture;
(2) reacting the first mixture in a beaker at the temperature of 95 ℃ for 2 hours, and naturally cooling to room temperature to obtain a second mixture;
(3) standing the second mixture for 20 hours, then carrying out vacuum filtration, and heating the obtained precipitate in an oven at 100 ℃ to a constant weight state (removing water) to obtain a third mixture;
(4) and calcining the third mixture in a muffle furnace at 650 ℃ for 3 hours, naturally cooling to room temperature, and grinding to obtain the Ce-Nb-O composite metal oxide catalyst which is marked as catalyst D.
Example 5: a method for synthesizing a Ce-Nb-O composite metal oxide catalyst comprises the following steps:
(1) adding 50mL of deionized water into a 250mL beaker, then adding a certain amount of cerous nitrate, niobium oxalate and urea, and stirring to uniformly mix the cerous nitrate, the niobium oxalate and the urea, wherein the dosage ratio of metal elements in the niobium oxalate to the deionized water, the urea and the cerous nitrate is 0.1 mol: 50mL of: 4 mol: 0.1mol to obtain a first mixture;
(2) reacting the first mixture in a beaker at 75 ℃ for 5 hours, and then naturally cooling to room temperature to obtain a second mixture;
(3) standing the second mixture for 16 hours, then carrying out vacuum filtration, and heating the obtained precipitate in an oven at 90 ℃ to a constant weight state (removing water) to obtain a third mixture;
(4) and calcining the third mixture in a muffle furnace at 700 ℃ for 2 hours, naturally cooling to room temperature, and grinding to obtain the Ce-Nb-O composite metal oxide catalyst marked as catalyst E.
Application of Ce-Nb-O composite metal oxide catalyst
Examples 6 to 10
The catalysts A to E prepared in examples 1 to 5 were used for catalytic combustion of different organic waste gases with a concentration of 1000ppmv respectively (the organic waste gases were single toluene, single monochlorobenzene, single chloroethylene or a mixture of toluene, monochlorobenzene and chloroethylene respectively occupying 1/3, the balance gas was dry air, and the gas space velocity was 104mLgas h-1gcat.-1The gas flow rate was 80 mL/min). Specific parametric indicators for 99.5% conversion of the reactants achieved by each catalyst are shown in table 1. Through further determination, the Ce-Nb-O composite metal oxide catalyst can realize the complete catalytic degradation of the pollutants at the temperature below 300 ℃.
The combustion product of the catalytic reaction of the organic waste gas containing the single toluene is determined to be H2O、COx(wherein CO)2Selectivity > 85%), and combustion products of other organic exhaust gas catalytic reactions are H2O, HCl and COx(wherein CO)2Selectivity was > 85% and HCl selectivity > 99%), no other by-products were detected using a gas chromatograph equipped with TCD and FID detectors.
TABLE 1 reaction temperature (. degree.C.) required for each catalyst to achieve a 1000ppmv organic waste gas degradation of 99.5%
Examples 11 to 15
The catalysts A to E prepared in examples 1 to 5 were used for catalytic combustion of different organic waste gases with a concentration of 1000ppmv respectively (the organic waste gases were single toluene, single monochlorobenzene, single chloroethylene or a mixture of toluene, monochlorobenzene and chloroethylene respectively occupying 1/3, the balance gas was dry air, and the gas space velocity was 104mLgas h-1gcat.-1And the gas flow is 80mL/min), during catalytic combustion, firstly heating to 700 ℃ for reaction for 1h, then cooling to 300 ℃ for continuous reaction, and testing the catalytic degradation rate before and after cooling. The test result shows that the catalytic effect of each catalyst is not reduced when the catalytic degradation rate at 700 ℃ is compared with that at 300 ℃, which shows that the catalytic material synthesized by the synthesis method has good service life and can resist high-temperature thermal shock at 700 ℃ in a short period.
Examples 16 to 20
The catalysts A to E prepared in examples 1 to 5 were used for catalytic combustion of different organic waste gases each having a concentration of 1000ppmv (organic combustion)The waste gas is single toluene, single monochlorobenzene, single chloroethylene or the mixture gas of toluene, monochlorobenzene and chloroethylene respectively occupying 1/3, the balance gas is dry air, and the gas space velocity is 104mLgas h-1gcat.-1And the gas flow is 80mL/min), the temperature is raised to 300 ℃ during catalytic combustion, the reaction is continued for 168 hours, and the catalytic activity of the catalyst is tested every 4 hours. The test result shows that the catalytic activity of each catalyst is not obviously reduced in the process of continuously reacting for 168 hours.
Examples 21 to 25
The catalysts A to E prepared in examples 1 to 5 were used for catalytic combustion of organic waste gases having a concentration of 1000ppmv (the organic waste gases were toluene alone, monochlorobenzene alone, vinyl chloride alone, or a mixture of toluene, monochlorobenzene, and vinyl chloride each in 1/3, and the balance gas was 20% O)2Ar at a gas space velocity of 104mLgas h-1gcat.-1And the gas flow is 80mL/min), and a GC-MS combined instrument is adopted to detect the concentration of each substance at the gas inlet and the gas outlet on line.
The specific operation process is as follows: the catalyst is firstly treated at 300 ℃ and 20% of O2Pretreating in Ar for 30 min; cooling to 50 deg.C, when the VOCs is 1000ppmv (20% O as balance gas)2After the/Ar) reaches the adsorption-desorption equilibrium on the surface of the catalyst, the temperature is raised to 500 ℃ at the speed of 5 ℃/min, and the reactants and the final product (CO) are tracked on line by utilizing GC-MS in the process2/CO，Cl2HCl and H2O) and possible by-products (e.g. CH)3Cl、C2H3Cl、HCHO、CH3CHO、CH3COOH) concentration. The test result shows that CO is removed in the catalytic reaction processxHCl and H2Besides O, no other by-products were detected.
Examples 26 to 30
The catalysts A to E prepared in examples 1 to 5 were used for catalytic combustion of organic waste gases having a concentration of 1000ppmv (the organic waste gases were toluene alone, monochlorobenzene alone, vinyl chloride alone, or a mixture of toluene, monochlorobenzene, and vinyl chloride each in 1/3, and the balance gas was 20％O2Ar at a gas space velocity of 104mLgas h-1gcat.-1And the gas flow is 80mL/min), continuously reacting for 5h at 300 ℃ during catalytic combustion, absorbing tail gas by 10mL of diethylene glycol, and detecting and analyzing the obtained liquid by adopting a GC-MS instrument. The test results showed that no by-product was detected.
With the combination of the embodiments 6-30, the Ce-Nb-O composite metal oxide catalyst can completely catalyze and decompose three typical volatile organic compounds at a low reaction temperature (300 ℃), can resist high-temperature thermal shock of 700 ℃, can maintain good catalytic activity after reacting for 168 hours, and does not generate toxic and harmful byproducts.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A method for synthesizing a Ce-Nb-O composite metal oxide catalyst is characterized by comprising the following steps: the method comprises the following steps: uniformly mixing deionized water, cerium nitrate, niobium oxalate and urea in a beaker according to a proportion, and then stirring and heating for reaction; and after the reaction is finished, naturally cooling, standing, performing suction filtration, and drying and calcining the obtained precipitate to obtain the Ce-Nb-O composite metal oxide catalyst.
2. The method for synthesizing a Ce-Nb-O composite metal oxide catalyst according to claim 1, wherein: the dosage ratio of the metal elements in the niobium oxalate to the deionized water, the urea and the cerium nitrate is 0.1 mol: 50mL of: (4-22) mol: (0.1 to 1) mol.
3. The method for synthesizing a Ce-Nb-O composite metal oxide catalyst according to claim 1, wherein: the molar ratio of the sum of metal elements in the two raw materials of the cerium nitrate and the niobium oxalate to the urea is 1: 20.
4. the method for synthesizing a Ce-Nb-O composite metal oxide catalyst according to claim 1, wherein: the heating reaction temperature is 75-95 ℃, and the heating reaction time is 2-5 hours.
5. The method for synthesizing a Ce-Nb-O composite metal oxide catalyst according to claim 1, wherein: and naturally cooling the reacted mixture to room temperature, and then standing for 12-24 hours.
6. The method for synthesizing a Ce-Nb-O composite metal oxide catalyst according to claim 1, wherein: and the drying operation is to place the obtained precipitate in a drying oven and heat the precipitate to constant weight at the temperature of 90-120 ℃.
7. The method for synthesizing a Ce-Nb-O composite metal oxide catalyst according to claim 1, wherein: and the calcination operation is to place the dried powder in a muffle furnace for calcination for 2-5 hours at the temperature of 450-700 ℃.
8. The method for synthesizing a Ce-Nb-O composite metal oxide catalyst according to claim 1, wherein: the Ce-Nb-O composite metal oxide catalyst is prepared by compounding chemical elements Ce, Nb and O, wherein the molar ratio of the metal elements is Ce: nb (1-10): 1, and the balance of O element; the chemical composition of the Ce-Nb-O composite metal oxide catalyst can be represented as xCeO2-yNb2O5。
9. The application of the Ce-Nb-O composite metal oxide catalyst prepared by the synthesis method according to any one of claims 1 to 8 is characterized in that: the Ce-Nb-O composite metal oxide catalyst is applied to catalytic combustion of several typical VOCs and shows excellent catalytic degradation performance.
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