CN111822042A - Composite metal catalyst for online hydrocarbon removal instrument and preparation method thereof - Google Patents
Composite metal catalyst for online hydrocarbon removal instrument and preparation method thereof Download PDFInfo
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- CN111822042A CN111822042A CN202010397982.8A CN202010397982A CN111822042A CN 111822042 A CN111822042 A CN 111822042A CN 202010397982 A CN202010397982 A CN 202010397982A CN 111822042 A CN111822042 A CN 111822042A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/74—Noble metals
- B01J29/7476—MWW-type, e.g. MCM-22, ERB-1, ITQ-1, PSH-3 or SSZ-25
Abstract
The invention provides a composite metal catalyst for an online hydrocarbon removal instrument and a preparation method thereof, which are used for solving the technical problem of low catalytic efficiency of hydrocarbon substances of the online hydrocarbon removal instrument in the prior art, and comprise the following steps: s1: dissolving a template, Pd (NO3) 2.6H 2O and RuCl 3.3H 2O in a solvent I, and adding an alkaline solution to obtain a mixture; heating and separating to obtain a first solid; s2: adding the first solid, CTMAB, TEOS and the second solvent into a container, adding a precipitator for reaction, separating to obtain a second solid, and calcining the second solid to obtain PdxRuy/SiO2 nanoparticles; s3: the PdxRuy/SiO2 nano-particles, MCM-22 and water are processed into molecular sieve water slurry, the molecular sieve water slurry is covered on the surface of a carrier, and the composite metal catalyst is obtained by drying and calcining. The technical scheme of the invention is implemented by taking noble metals Pd and Ru as active components and SiO2And MCM-22 molecular sieve are evenly mixed, and finally the mixture is evenly coated on the surface of a zeolite carrier to prepare PdxRuy/SiO2the/MCM-22/Zeolite composite metal catalyst is effectively improvedThe catalytic decomposition efficiency of the online hydrocarbon removing instrument is improved.
Description
Technical Field
The invention relates to the field of catalysts and hydrocarbon catalysts, in particular to a composite metal catalyst for an online hydrocarbon removal instrument and a preparation method thereof.
Background
The online hydrocarbon removing instrument can monitor and remove hydrocarbon substances in real time, and is commonly used in chemical plants, oil refineries and other environments which are easy to leak VOCs. In the prior art, the common method for eliminating hydrocarbon substances is to carry out heating catalytic decomposition on the hydrocarbon substances, but the catalytic efficiency of the catalyst is low. Therefore, whether a high-efficiency catalyst suitable for an online hydrocarbon remover exists or not is a technical problem expected to be solved by the technical personnel in the field.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a composite metal catalyst for an online hydrocarbon removal instrument and a preparation method thereof, and the technical scheme of the invention is implemented as follows:
a preparation method of a composite metal catalyst for an online hydrocarbon removal instrument comprises the following steps:
s1: dissolving a template, Pd (NO3) 2.6H 2O and RuCl 3.3H 2O in a solvent I, and adding an alkaline solution to obtain a mixture; then heating and separating the mixture to obtain a first solid;
s2: adding the first solid, the CTMAB, the TEOS and a second solvent into a container, adding a precipitator for reaction, then separating to obtain a second solid, and calcining the second solid to obtain PdxRuy/SiO2 nanoparticles;
s3: the PdxRuy/SiO2 nano-particles, MCM-22 and water are processed into molecular sieve water slurry, the molecular sieve water slurry is covered on the surface of a carrier, and the composite metal catalyst is obtained by drying and calcining.
Preferably, in S1, the mole ratio of Pd to Ru is 0.5-2.
Preferably, in S1 and S2, the molar ratio of TEOS to Pd is 0.5-4, and the molar ratio of CTMAB to Pd is 0.5-4.
Preferably, the heating method in S1 is: heating with microwave oven for 30-60S.
Preferably, the separation method in S1 is: the mixture was cooled to room temperature and washed with water and dried at 45-75 ℃ to give a solid one.
Preferably, in S2, the calcination method is: calcining for 1-5 hours in a muffle furnace at 500-600 ℃.
Preferably, in S3, the drying method includes: drying in a vacuum drying oven at 60-100 deg.C for 3-6 hr;
in S3, the calcining method comprises the following steps: calcining for 2-8 hours in a muffle furnace at 400-700 ℃.
Preferably, in S1, the precipitant includes ammonia or urea.
Preferably, in S1, the alkaline solution includes n-butylamine, dimethylglyoxime, or ethylenediamine.
The invention also aims to provide a composite metal catalyst for the online hydrocarbon removal instrument, and the preparation method is a preparation method of the composite metal catalyst for the online hydrocarbon removal instrument with the characteristics.
By implementing the technical scheme of the invention, the technical problem of low hydrocarbon removal efficiency of the online hydrocarbon removal instrument in the prior art can be solved; the technical scheme of the invention is implemented by taking noble metals Pd and Ru as active components and SiO2And MCM-22 molecular sieve are evenly mixed, and finally the mixture is evenly coated on the surface of a zeolite carrier to prepare PdxRuy/SiO2the/MCM-22/Zeolite composite metal catalyst effectively improves the catalytic decomposition efficiency of the on-line hydrocarbon removal instrument.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
3.5g of template and 0.025mol of Pd (NO3) 2.6H 2O and 0.025mol of RuCl 3.3H 2O were dissolved in 10ml of ethylene glycol and the solution was slowly added dropwise to the solution. After mixing well, heating by microwave oven radiation, cooling to room temperature and washing with distilled water to obtain Pdx/Ruy and drying. The obtained Pdx/Ruy is added into a 500mL flask, 250mL of ethanol, 50mL of purified water, 10g of CTMAB and 5.0g of TEOS are added, ammonia water is added dropwise at 45 ℃ for stirring reaction for 6 hours, then the mixture is filtered, washed by water, vacuum-dried at 65 ℃, and finally calcined at 600 ℃ for 5 hours in a muffle furnace, and PdxRuy/SiO2 nanoparticles are obtained. 5.0g of PdxRuy/SiO2 nano-particles, 5.0g of MCM-22 and deionized water are treated on a ball mill for 1.5 to 3 hours to prepare molecular sieve water slurry. Then, under the vacuum state, the water slurry of the molecular sieve is evenly covered on the Zeolite surface. And finally, drying in a vacuum drying oven at 70 ℃, and calcining in a muffle furnace at 550 ℃ to obtain the PdxRuy/SiO2/MCM-22/Zeolite composite metal catalyst.
Example 2
3.5g of template and 0.025mol of Pd (NO3) 2.6H 2O and 0.025mol of RuCl 3.3H 2O were dissolved in 10ml of ethylene glycol and the solution was slowly added dropwise to the solution. After mixing well, heating by microwave oven radiation, cooling to room temperature and washing with distilled water to obtain Pdx/Ruy and drying. The obtained Pdx/Ruy is added into a 500mL flask, 250mL of ethanol, 50mL of purified water, 10g of CTMAB and 7.5g of TEOS are added, ammonia water is added dropwise at 45 ℃ for stirring reaction for 6 hours, then the mixture is filtered, washed by water, vacuum-dried at 65 ℃, and finally calcined at 600 ℃ for 5 hours in a muffle furnace, and PdxRuy/SiO2 nanoparticles are obtained. 5.0g of PdxRuy/SiO2 nano-particles, 5.0g of MCM-22 and deionized water are treated on a ball mill for 1.5 to 3 hours to prepare molecular sieve water slurry. Then, under the vacuum state, the water slurry of the molecular sieve is evenly covered on the Zeolite surface. And finally, drying in a vacuum drying oven at 70 ℃, and calcining in a muffle furnace at 550 ℃ to obtain the PdxRuy/SiO2/MCM-22/Zeolite composite metal catalyst.
Example 3
3.5g of template and 0.025mol of Pd (NO3) 2.6H 2O and 0.025mol of RuCl 3.3H 2O were dissolved in 10ml of ethylene glycol and the solution was slowly added dropwise to the solution. After mixing well, heating by microwave oven radiation, cooling to room temperature and washing with distilled water to obtain Pdx/Ruy and drying. The obtained Pdx/Ruy is added into a 500mL flask, 250mL of ethanol, 50mL of purified water, 10g of CTMAB and 10.0g of TEOS are added, ammonia water is added dropwise at 45 ℃ for stirring reaction for 6 hours, then the mixture is filtered, washed by water, vacuum-dried at 65 ℃, and finally calcined in a muffle furnace at 600 ℃ for 5 hours, so that PdxRuy/SiO2 nanoparticles are obtained. 5.0g of PdxRuy/SiO2 nano-particles, 5.0g of MCM-22 and deionized water are treated on a ball mill for 1.5 to 3 hours to prepare molecular sieve water slurry. Then, under the vacuum state, the water slurry of the molecular sieve is evenly covered on the Zeolite surface. And finally, drying in a vacuum drying oven at 70 ℃, and calcining in a muffle furnace at 550 ℃ to obtain the PdxRuy/SiO2/MCM-22/Zeolite composite metal catalyst.
Example 4
3.5g of template and 0.025mol of Pd (NO3) 2.6H 2O and 0.025mol of RuCl 3.3H 2O were dissolved in 10ml of ethylene glycol and the solution was slowly added dropwise to the solution. After mixing well, heating by microwave oven radiation, cooling to room temperature and washing with distilled water to obtain Pdx/Ruy and drying. The obtained Pdx/Ruy is added into a 500mL flask, 250mL of ethanol, 50mL of purified water, 10g of CTMAB and 7.5g of TEOS are added, ammonia water is added dropwise at 45 ℃ for stirring reaction for 6 hours, then the mixture is filtered, washed by water, vacuum-dried at 65 ℃, and finally calcined at 600 ℃ for 5 hours in a muffle furnace, and PdxRuy/SiO2 nanoparticles are obtained. 5.0g of PdxRuy/SiO2 nano-particles, 3.5g of MCM-22 and deionized water are treated on a ball mill for 1.5 to 3 hours to prepare molecular sieve water slurry. Then, under the vacuum state, the water slurry of the molecular sieve is evenly covered on the Zeolite surface. And finally, drying in a vacuum drying oven at 70 ℃, and calcining in a muffle furnace at 550 ℃ to obtain the PdxRuy/SiO2/MCM-22/Zeolite composite metal catalyst.
Example 5
3.5g of template and 0.025mol of Pd (NO3) 2.6H 2O and 0.025mol of RuCl 3.3H 2O were dissolved in 10ml of ethylene glycol and the solution was slowly added dropwise to the solution. After mixing well, heating by microwave oven radiation, cooling to room temperature and washing with distilled water to obtain Pdx/Ruy and drying. The obtained Pdx/Ruy is added into a 500mL flask, 250mL of ethanol, 50mL of purified water, 10g of CTMAB and 7.5g of TEOS are added, ammonia water is added dropwise at 45 ℃ for stirring reaction for 6 hours, then the mixture is filtered, washed by water, vacuum-dried at 65 ℃, and finally calcined at 600 ℃ for 5 hours in a muffle furnace, and PdxRuy/SiO2 nanoparticles are obtained. 5.0g of PdxRuy/SiO2 nano-particles, 2.5g of MCM-22 and deionized water are treated on a ball mill for 1.5 to 3 hours to prepare molecular sieve water slurry. Then, under the vacuum state, the water slurry of the molecular sieve is evenly covered on the Zeolite surface. And finally, drying in a vacuum drying oven at 70 ℃, and calcining in a muffle furnace at 550 ℃ to obtain the PdxRuy/SiO2/MCM-22/Zeolite composite metal catalyst.
Then, the catalyst of the PdxRuy/SiO2/MCM-22/Zeolite composite metal catalyst obtained in the example 1-5 is filled in a fixed bed reactor with the diameter of 2cm and the length of 4cm, the reaction is carried out under the conditions that the reaction temperature is 400 ℃, the pressure is 0.7Mpa and the volume space velocity is 0.1h < -1 >, and the gas chromatography detection is carried out until the reaction is finished. The concentrations of the components in the test gas were 10.1X 10-6 for benzene (35.1mg/m3), 10.6X 10-6 for toluene (43.6mg/m3), 9.1X 10-6 for o-xylene (43.1mg/m3), 10.0X 10-6 for methane (7.14mg/m3) and 10.0X 10-6 for methane (19.7mg/m3), with the remainder being nitrogen.
TABLE 1 catalyst compositions and catalytic efficiencies for examples 1-5
Comparative example 1
0.025mol of Pd (NO3) 2.6H 2O was added to a 500mL flask and 250mL of ethanol, 50mL of purified water, 10g of CTMAB, 10.0g of TEOS were added, ammonia was added dropwise at 45 ℃ and the mixture was stirred for 6 hours and then filtered, washed with water, vacuum-dried at 65 ℃ and finally calcined at 600 ℃ for 5 hours in a muffle furnace to obtain Pd/SiO2 nanoparticles.
Comparative example 2
0.025mol of RuCl3 & 3H2O was added to a 500mL flask and 250mL of ethanol, 50mL of purified water, 10g of CTMAB, 10.0g of TEOS were added, ammonia was added dropwise at 45 ℃ and stirred to react for 6 hours, then the mixture was filtered, washed with water, vacuum-dried at 65 ℃ and finally calcined at 600 ℃ for 5 hours in a muffle furnace to obtain Ru/SiO2 nanoparticles.
Comparative example 3
0.025mol of Pd (NO3) 2.6H 2O is added into a beaker, 5.0g of MCM-22 molecular sieve is added, and the mixture is dried in an oven at the temperature of 95 ℃ to obtain Pd/MCM-22.
Comparative example 4
0.025mol of Pd (NO3) 2.6H 2O is added into a beaker, 5.0g of MCM-22 molecular sieve is added, and the mixture is dried in an oven at the temperature of 95 ℃ to obtain Pd/MCM-22.
Comparative example 5
3.5g of template and 0.025mol of Pd (NO3) 2.6H 2O and 0.025mol of RuCl 3.3H 2O were dissolved in 10ml of ethylene glycol and the solution was slowly added dropwise to the solution. After mixing well, heating by microwave oven radiation, cooling to room temperature and washing with distilled water to obtain Pdx/Ruy and drying. The obtained Pdx/Ruy is added into a 500mL flask, 250mL of ethanol, 50mL of purified water, 10g of CTMAB and 10.0g of TEOS are added, ammonia water is added dropwise at 45 ℃ for stirring reaction for 6 hours, then the mixture is filtered, washed by water, vacuum-dried at 65 ℃, and finally calcined in a muffle furnace at 600 ℃ for 5 hours, so that PdxRuy/SiO2 nanoparticles are obtained.
Comparative example 6
3.5g of template and 0.025mol of Pd (NO3) 2.6H 2O and 0.025mol of RuCl 3.3H 2O were dissolved in 10ml of ethylene glycol and the solution was slowly added dropwise to the solution. After mixing well, heating by microwave oven radiation, cooling to room temperature and washing with distilled water to obtain Pdx/Ruy and drying. And adding the obtained PdxRuy nano-particles into a beaker, adding 5.0g of MCM-22 molecular sieve, and drying in a drying oven at the temperature of 95 ℃ to obtain PdxRuy/MCM-22.
Then filling the catalyst obtained in the comparative examples 1-6 into a fixed bed reactor with the diameter of 2cm and the length of 4cm, carrying out reaction under the conditions of reaction temperature of 400 ℃, pressure of 0.7Mpa and volume space velocity of 0.1h < -1 >, and detecting by gas chromatography until the reaction is finished. The concentrations of the components in the test gas were 10.1X 10-6 for benzene (35.1mg/m3), 10.6X 10-6 for toluene (43.6mg/m3), 9.1X 10-6 for o-xylene (43.1mg/m3), 10.0X 10-6 for methane (7.14mg/m3) and 10.0X 10-6 for methane (19.7mg/m3), with the remainder being nitrogen.
TABLE 2 catalyst compositions and catalytic efficiencies of comparative examples 1-6
According to the data, the catalyst prepared by the method has better catalysis effect on VOCs gas.
It should be understood that the above-described embodiments are merely exemplary of the present invention, and are not intended to limit the present invention, and that any modification, equivalent replacement, or improvement made without departing from the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a composite metal catalyst for an online hydrocarbon removal instrument is characterized by comprising the following steps:
s1: template and Pd (NO)3)2·6H2O and RuCl3·3H2Dissolving O in the first solvent, and adding an alkaline solution to obtain a mixture; then heating and separating the mixture to obtain a first solid;
s2: adding the first solid, CTMAB, TEOS and a second solvent into a container, adding a precipitator for reaction, separating to obtain a second solid, and calcining the second solid to obtain PdxRuy/SiO2A nanoparticle;
s3: pd is addedxRuy/SiO2And (3) processing the nano particles, MCM-22 and water into molecular sieve water slurry, covering the surface of the carrier with the molecular sieve water slurry, drying and calcining to obtain the composite metal catalyst.
2. The method for preparing a composite metal catalyst for an on-line hydrocarbon removal instrument as claimed in claim 1, wherein the molar ratio of Pd and Ru in S1 is 0.5-2.
3. The method of claim 1, wherein the molar ratio of TEOS to Pd is 0.5-4 and the molar ratio of CTMAB to Pd is 0.5-4 in S1 and S2.
4. The preparation method of the composite metal catalyst for the online hydrocarbon removal instrument as claimed in claim 1, wherein the heating method in S1 is as follows: heating with microwave oven for 30-60S.
5. The preparation method of the composite metal catalyst for the online hydrocarbon removal instrument as claimed in claim 1, wherein the separation method in S1 is as follows: the mixture was cooled to room temperature and washed with water and dried at 45-75 ℃ to give a solid one.
6. The method for preparing the composite metal catalyst for the on-line hydrocarbon removal instrument as claimed in claim 1, wherein in S2, the calcination method comprises: calcining for 1-5 hours in a muffle furnace at 500-600 ℃.
7. The preparation method of the composite metal catalyst for the on-line hydrocarbon removal instrument according to claim 1, wherein in S3, the drying method comprises the following steps: drying in a vacuum drying oven at 60-100 deg.C for 3-6 hr;
in S3, the calcining method comprises the following steps: calcining for 2-8 hours in a muffle furnace at 400-700 ℃.
8. The method of claim 1, wherein in S1, the precipitant comprises ammonia or urea.
9. The method for preparing the composite metal catalyst for the on-line hydrocarbon removal instrument as recited in claim 1, wherein in the S1, the alkaline solution comprises n-butylamine, dimethylglyoxime, or ethylenediamine.
10. The composite metal catalyst for the online hydrocarbon removal instrument is characterized by being prepared according to the preparation method of the composite metal catalyst for the online hydrocarbon removal instrument of any one of claims 1 to 9.
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