CN107876060B - Cerium-cobalt catalyst for complete oxidation of propane and preparation method and application thereof - Google Patents
Cerium-cobalt catalyst for complete oxidation of propane and preparation method and application thereof Download PDFInfo
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- CN107876060B CN107876060B CN201711045069.6A CN201711045069A CN107876060B CN 107876060 B CN107876060 B CN 107876060B CN 201711045069 A CN201711045069 A CN 201711045069A CN 107876060 B CN107876060 B CN 107876060B
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
Abstract
The invention discloses a cerium-cobalt catalyst for completely oxidizing propane and a preparation method and application thereof, belonging to the technical field of catalyst synthesis and application. The cobalt salt and the cerium salt are added into a tertiary butanol solution containing inorganic acid, polyether surfactant and sodium dodecyl sulfate, stirred until the cobalt salt and the cerium salt are completely dissolved, then the mixture is placed at the temperature of 20-70 ℃ for reaction for 1-3 hours, and then the mixture is frozen, dried and roasted to obtain the cerium cobalt catalyst for completely oxidizing propane. Compared with the conventional catalyst, the catalyst has the advantages of high activity, low cost, high stability and the like, and the catalytic activity and the stability of the catalyst are well improved through the synergistic effect of Co and Ce. The cerium cobalt catalyst of the invention can realize the complete removal of pollutants at the temperature of below 300 ℃.
Description
Technical Field
The invention relates to the technical field of catalyst synthesis and application, in particular to a cerium-cobalt catalyst suitable for complete oxidation of propane, a preparation method thereof and application in the field of volatile pollutant purification.
Background
With the annual increase of the motor vehicle keeping amount in China, the urban air quality is gradually deteriorated, and the motor vehicle tail gas control has been widely concerned. The motor vehicle tail gas mainly refers to particulate matters, CO and NOxAnd Hydrocarbons (HC), and the like. As an important volatile organic compound, HC can cause a series of ecological environmental problems such as photochemical smog, dust-haze weather, ozone layer damage and the like, and seriously threatens human health. Compared with other mobile source pollutants, HC has the characteristics of multiple types, difficult degradation, high toxicity and the like. Therefore, how to purify HC efficiently has been a difficult and critical issue in current research.
The mainstream technologies for HC treatment mainly include adsorption and catalytic oxidation methods. However, the former has problems that adsorption is easily saturated, secondary pollution is uncontrollable, and regeneration is difficult. The catalytic oxidation method has the advantages of high waste gas treatment efficiency, high safety, low energy consumption, low secondary pollution and the like, and is one of the most researched and widely used VOCs treatment measures at present. The main principle is as follows: under the action of catalyst, the pollutant is decomposed completely at relatively low temperature and converted into harmless gas. Therefore, how to select the high-efficiency and low-cost catalyst is the core and key of the catalytic oxidation technology. For HC compounds with stable structures, the temperature of over 300 ℃ is usually needed for complete catalytic oxidation, and besides the expensive noble metal catalyst, the conventional perovskite and hydrotalcite catalysts are difficult to realize efficient removal of pollutants at lower temperature. Therefore, it is of great significance to develop a high-efficiency, low-cost HC catalytic oxidation catalyst.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a cerium-cobalt catalyst for completely oxidizing propane and a preparation method thereof, which can be used for HC oxidation and other VOCs elimination.
The invention relates to a preparation method of a cerium-cobalt catalyst for completely oxidizing propane, which comprises the following steps:
firstly, adding a cobalt salt and a cerium salt into a tertiary butanol solution containing an inorganic acid, a polyether surfactant and Sodium Dodecyl Sulfate (SDS) according to a molar ratio of Co/(Ce + Co) of 0-1, stirring until the cobalt salt and the cerium salt are completely dissolved, and then reacting for 1-3 hours at 20-70 ℃ to obtain a mixed solution.
And secondly, placing the obtained mixed solution in a liquid nitrogen environment for quick freezing, and then placing the mixed solution in a low-temperature refrigerator for continuous freezing and compaction for later use.
And step three, freezing and drying the substance frozen and compacted in the step two to obtain a semi-finished product.
And fourthly, roasting the semi-finished product in the third step for 12 hours at 150 ℃ in air to remove the undecomposed surfactant and other residues, and then continuously raising the temperature to the target temperature. Thus obtaining the cerium cobalt catalyst for the complete oxidation of propane.
The cerium salt is trivalent or quadrivalent cerium salt containing crystal water, and can be cerium chloride, cerium nitrate, ammonium cerium nitrate and cerium sulfate, preferably cerium nitrate; the cobalt salt is divalent cobalt salt containing crystal water, and can be cobalt sulfate, cobalt nitrate, cobalt chloride and cobalt acetylacetonate, and cobalt nitrate is preferred; the inorganic acid can be nitric acid, sulfuric acid and hydrochloric acid, preferably nitric acid; the polyether surfactant may be P123, F108 and F127, preferably P123.
In the mixed solution, the molar ratio of the transition metal salt to the inorganic acid is 2-10; the mass ratio of the transition metal salt to the polyether surfactant is 1-10; the molar ratio of the tert-butyl alcohol to the transition metal salt is 10-50, wherein the transition metal salt refers to the sum of cobalt salt and cerium salt.
The cerium-cobalt catalyst for the complete oxidation of propane prepared by the method can be applied to the complete catalytic oxidation of hydrocarbons such as propane, propylene, methane and the like and the purification of other VOCs. The method specifically comprises the following steps:
(1) the cerium-cobalt catalyst is loaded into a micro fixed bed reactor, and the reaction temperature is controlled to be 150-350 ℃;
(2) the flow rate of the gas is controlled to be 100mL/min, the oxygen content is 20 percent, the water content is 2 percent, and the space velocity can be controlled to be 60000mL g-1h-1。
Compared with the conventional catalyst, the catalyst has the advantages of high activity, low cost, high stability and the like, the optimal ratio of cerium to cobalt is 2:3, and the catalytic activity and stability of the catalyst are well improved through the synergistic effect of Co and Ce. The cerium cobalt catalyst of the invention can realize the complete removal of pollutants at the temperature of below 300 ℃.
Drawings
Fig. 1 is a high angle annular dark field image photograph of the cerium cobalt catalyst prepared in example 4.
Fig. 2 is an energy spectrum of the high angle annular dark field image shown in fig. 1.
Detailed Description
Example 1Co1Ce4And (3) preparing a catalyst.
(1) Dissolving 3g P123, 0.1g SDS and 2mL nitric acid in 20mL tertiary butanol solvent, stirring and mixing to obtain alcoholic solution;
(2) dissolving 6.95g of cerous nitrate hexahydrate and 1.16g of cobaltous nitrate tetrahydrate in the alcohol solution in the step (1), and stirring at room temperature for 60 min;
(3) stirring the mixed solution at 60 ℃ for reaction for 3h, then freezing the mixed solution in a liquid nitrogen environment for 5min, and then freezing the mixed solution in a-50 ℃ environment for more than 12 h;
(4) freeze-drying the substance prepared in the step (3) to obtain a semi-finished product;
(5) and (4) placing the semi-finished product obtained in the step (4) into a tube furnace, roasting for 12 hours at the temperature of 150 ℃, then raising the temperature to 350 ℃ at the speed of 2 ℃/min and keeping for 2-4 hours to obtain the novel cerium-cobalt composite oxide catalyst.
Example 2Co2Ce3And (3) preparing a catalyst.
(1) Dissolving 3g P123, 0.1g SDS and 2mL nitric acid in 20mL tertiary butanol solution, stirring and mixing to obtain alcoholic solution;
(2) dissolving 5.21g of cerium nitrate and 2.33g of cobalt nitrate into the alcoholic solution in the step (1), and stirring at room temperature for 60 min;
(3) stirring the mixed solution at 70 ℃ for reaction for 1h, then freezing the mixed solution in a liquid nitrogen environment for 5min, and then freezing the mixed solution in a-50 ℃ environment for more than 12 h;
(4) freeze-drying the substance prepared in the step (3) to obtain a semi-finished product;
(5) and (4) placing the semi-finished product obtained in the step (4) into a tubular furnace, roasting for 12 hours at the temperature of 150 ℃, and then raising the temperature to 350 ℃ at the speed of 2 ℃/min to obtain the novel cerium-cobalt composite oxide catalyst.
Example 3Co1Ce1Preparation of samples
(1) 3g P123, 0.1g SDS and 2mL nitric acid are dissolved in 20mL tertiary butanol solution and stirred and mixed;
(2) dissolving 4.32g of cerium nitrate and 2.91g of cobalt nitrate into the alcoholic solution in the step (1), and stirring at room temperature for 60 min;
(3) stirring the mixed solution at 20 ℃ for reaction for 3h, then freezing the mixed solution in a liquid nitrogen environment for 5min, and then freezing the mixed solution in a-50 ℃ environment for more than 12 h;
(4) freeze-drying the substance obtained in the step (3) to obtain a semi-finished product;
(5) and (3) putting the semi-finished product obtained in the step (4) into a tubular furnace, roasting for 12 hours at the temperature of 150 ℃, and then raising the temperature to 350 ℃ at the speed of 2 ℃/min and keeping for 2-4 hours to obtain the novel cerium-cobalt composite oxide catalyst.
Example 4Co3Ce2And (3) preparing a catalyst.
(1) 3g P123, 0.1g SDS and 2mL nitric acid are dissolved in 20mL tertiary butanol solution and stirred and mixed;
(2) dissolving 3.47g of cerium nitrate and 3.49g of cobalt nitrate into the alcoholic solution in the step (1), and stirring at room temperature for 60 min;
(3) stirring the mixed solution at 60 ℃ for reaction for 2h, then placing the solution in a liquid nitrogen environment for freezing for 5min, and then placing the solution in a-50 ℃ environment for freezing for 12 h;
(4) freeze-drying the substance obtained in the step (3) to obtain a semi-finished product;
(5) and (3) putting the semi-finished product obtained in the step (4) into a tubular furnace, roasting for 12 hours at the temperature of 150 ℃, and then raising the temperature to 350 ℃ at the speed of 2 ℃/min and keeping for 2-4 hours to obtain the novel cerium-cobalt composite oxide catalyst.
Co as shown in FIGS. 1 and 23Ce2The prepared cerium-cobalt catalyst has a developed mesoporous structure, the aperture range is 2-5nm, cobalt and cerium in the catalyst are crosslinked in a worm-like particle structure, and the direct relationship is realized with micelles formed by using a surfactant for induction. The developed pore structure and smaller oxide particle size of the catalyst should be the key to its high specific surface area and high conversion efficiency. In addition, the mapping result shown in fig. 2 shows that the elements are uniformly distributed, which indicates that the preparation method can realize uniform dispersion of the precursors of the two transition metal compounds, and this is also beneficial to the catalyst reaction.
Example 5Co4Ce1And (3) preparing a catalyst.
(1) 3g P123, 0.1g SDS and 2mL nitric acid are dissolved in 20mL tertiary butanol solution and stirred and mixed;
(2) dissolving 1.74g of cerium nitrate and 4.66g of cobalt nitrate into the alcoholic solution in the step (1), and stirring at room temperature for 60 min;
(3) stirring the mixed solution at 60 ℃ for reaction for 3h, then placing the solution in a liquid nitrogen environment for freezing for 5min, and then placing the solution in a-50 ℃ environment for freezing for 12 h;
(4) freeze-drying the substance obtained in the step (3) to obtain a semi-finished product;
(5) and (3) putting the semi-finished product obtained in the step (4) into a tube furnace, roasting for 12h at the temperature of 150 ℃, and then raising the temperature to 350 ℃ at the speed of 2 ℃/min and keeping for 2-4h to obtain the novel cerium-cobalt catalyst.
When the molar ratio of Co/(Ce + Co) was 0, the amount of Co added was 0, and a Ce catalyst was obtained by the preparation method of example 1, and when the molar ratio of Co/(Ce + Co) was 1, the amount of Ce added was 0, and a Co catalyst was obtained by the preparation method of example 1.
Application example 1:
the activity of the catalyst was evaluated in a quartz tube reactor having an inner diameter of 6mm and a length of 300 mm. The catalyst is prepared from 6000ppm propane and 20% O2，2％H2O, the residual gas is N2Under the reaction conditions of (1), the using amount of the catalyst is 0.1g, and the reaction space velocity is 60000ml g-1h-1. The results of the catalytic performance tests are shown in table 1.
TABLE 1 catalytic performance for complete oxidation of propane of cerium-cobalt composite oxides
Table 1 shows that of the six catalysts, Co3Ce2The activity of the complete catalytic oxidation reaction of the propane is highest; the reaction activity sequence is as follows:
Co3Ce2>Co1Ce1>Co4Ce1>Co2Ce3>Co>Co1Ce4。
the applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a cerium cobalt catalyst for the complete oxidation of propane is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
firstly, according to the proportion that the molar ratio of Co/(Ce + Co) is less than 1 and the proportion value does not include 0 and 1, adding cobalt salt and cerium salt into a tertiary butanol solution containing inorganic acid, polyether surfactant and lauryl sodium sulfate, stirring until the cobalt salt and the cerium salt are completely dissolved, and then reacting for 1-3 hours at the temperature of 20-70 ℃ to obtain a mixed solution; the polyether surfactant is any one of P123, F108 and F127;
secondly, placing the obtained mixed solution in a liquid nitrogen environment for quick freezing, and then placing the mixed solution in a low-temperature refrigerator for continuous freezing and compaction for later use;
step three, freezing and drying the substance frozen and compacted in the step two to obtain a semi-finished product;
fourthly, roasting the semi-finished product in the third step for 12 hours at 150 ℃ in the air, then continuously heating to the target temperature and keeping the temperature for 2-4 hours to obtain the cerium-cobalt catalyst for completely oxidizing the propane; the prepared cerium-cobalt catalyst has a developed mesoporous structure, the aperture range is 2-5nm, cobalt and cerium in the catalyst are crosslinked in a worm-shaped particle structure, and Co and Ce elements are alternated and uniformly distributed.
2. The method for preparing a cerium cobalt catalyst for the complete oxidation of propane according to claim 1, wherein: the cerium salt is trivalent or quadrivalent cerium salt containing crystal water, the cobalt salt is divalent cobalt salt containing crystal water, and the inorganic acid is any one of nitric acid, sulfuric acid or hydrochloric acid.
3. The method for preparing a cerium cobalt catalyst for the complete oxidation of propane according to claim 1, wherein: the cerium salt is any one of cerium chloride, cerium nitrate and cerium sulfate containing crystal water, and the cobalt salt is any one of cobalt sulfate, cobalt nitrate, cobalt chloride and cobalt acetylacetonate containing crystal water.
4. The method for preparing a cerium cobalt catalyst for the complete oxidation of propane according to claim 1, wherein: the cerium salt is cerous nitrate hexahydrate, and the cobalt salt is cobalt nitrate tetrahydrate; the inorganic acid is nitric acid; the polyether surfactant is P123.
5. The method for preparing a cerium cobalt catalyst for the complete oxidation of propane according to claim 1, wherein: in the mixed solution in the first step, the molar ratio of the transition metal salt to the inorganic acid is 2-10; the mass ratio of the transition metal salt to the polyether surfactant is 1-10; the molar ratio of the tert-butyl alcohol to the transition metal salt is 10-50, wherein the transition metal salt refers to the sum of cobalt salt and cerium salt.
6. The method for preparing a cerium cobalt catalyst for the complete oxidation of propane according to claim 1, wherein: and in the second step, the mixture is placed in a low-temperature refrigerator for continuous freezing compaction, specifically, the mixture is frozen for more than 12 hours in an environment with the temperature of 50 ℃ below zero.
7. The method for preparing a cerium cobalt catalyst for the complete oxidation of propane according to claim 1, wherein: the target temperature in the fourth step is 350 ℃.
8. The method for preparing a cerium cobalt catalyst for the complete oxidation of propane according to claim 1, wherein: the temperature rising rate of the continuous temperature rising in the fourth step is 2 ℃/min.
9. A cerium cobalt catalyst for the complete oxidation of propane, characterized in that: prepared by the preparation method of any one of claims 1 to 8; the prepared cerium-cobalt catalyst has a developed mesoporous structure, the aperture range is 2-5nm, cobalt and cerium in the catalyst are crosslinked in a worm-shaped particle structure, and Co and Ce elements are alternated and uniformly distributed.
10. A cerium cobalt catalyst for the complete oxidation of propane, characterized in that: the method is applied to the complete catalytic oxidation of propane, propylene and methane and the purification of VOCs, and specifically comprises the following steps:
(1) the cerium-cobalt catalyst is loaded into a micro fixed bed reactor, and the reaction temperature is controlled to be 150-350 ℃; the cerium-cobalt catalyst is prepared by any one preparation method of claims 1-8;
(2) controlling the flow rate of the gas to be 100mL/min, the oxygen content to be 20 percent, the water content to be 2 percent and the residual gas to be N2Under the reaction condition of (1), the space velocity is controlled to be 60000ml g-1h-1。
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