CN115739194A - Method for catalytic combustion of solvent oil by using MOFs (metal-organic frameworks) derived chromium-based catalyst loaded with monatomic platinum - Google Patents
Method for catalytic combustion of solvent oil by using MOFs (metal-organic frameworks) derived chromium-based catalyst loaded with monatomic platinum Download PDFInfo
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 87
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 44
- 239000011651 chromium Substances 0.000 title claims abstract description 44
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 43
- 238000007084 catalytic combustion reaction Methods 0.000 title claims abstract description 39
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- 239000012855 volatile organic compound Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
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- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- GVHCUJZTWMCYJM-UHFFFAOYSA-N chromium(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GVHCUJZTWMCYJM-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 238000002360 preparation method Methods 0.000 claims description 9
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- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000013178 MIL-101(Cr) Substances 0.000 claims description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
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- 230000000694 effects Effects 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention provides a method for catalytic combustion of solvent oil by using a MOFs (metal organic frameworks) derived chromium-based catalyst loaded with monatomic platinum, which comprises the steps of uniformly mixing deionized water, nonahydrate chromium nitrate, terephthalic acid, chloroplatinic acid and 40% hydrofluoric acid, transferring the mixture into a lining of a high-pressure reaction kettle, carrying out ultrasonic treatment, carrying out hydrothermal reaction for 8 hours at 220 ℃, obtaining dark green suspension, carrying out centrifugal washing on the obtained dark green suspension, drying the obtained product overnight at 80 ℃, and roasting the obtained product for 3 hours in a muffle furnace at 450 ℃ to obtain the MOFs derived chromium-based catalyst loaded with monatomic platinum; the obtained catalyst is loaded into a tubular reactor, solvent oil and air are mixed and blown into the tubular reactor in a bubbling mode, and the catalytic combustion reaction is carried out for 2 to 24 hours at the temperature of between 120 and 240 ℃. The MOFs-derived chromium-based catalyst loaded with monatomic platinum of the inventionThe solvent oil is catalyzed and combusted under the condition of no external oxygen supply, and the target product CO is generated at low temperature, high efficiency and high selectivity 2 And the method generates non-toxic byproducts, and can be applied to the degradation of low-concentration VOCs in large-scale chemical plants.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a method for catalyzing and combusting solvent oil by using a MOFs-derived chromium-based catalyst loaded with monatomic platinum.
Background
Volatile Organic Compounds (VOCs) are mainly emitted in solvent evaporation, chemical production processes and irregular human activities. In many industrial processes, such as petrochemical, automobile exhaust, electronic semiconductor and chemical pharmaceutical industries, a large amount of VOCs are emitted every year. Due to the toxicity and biostability of VOCs, their emissions pose serious risks to the environment and public health. Currently, many efforts have been made to reduce or eliminate the emission of VOCs, wherein the main methods include adsorption method, catalytic combustion method, absorption method, etc., wherein the cost of the adsorbent in the adsorption method is high, the recovery of the adsorbent in the absorption method also affects the economic efficiency, and the catalytic combustion method has the advantages of less by-products, relatively low temperature in practical application, etc. and is receiving much attention.
When the size of the catalyst material is in a nanometer level, various effects such as a surface (interface) effect, a small-size effect, a quantum size effect, a dielectric confinement effect, a macroscopic quantum tunneling effect and the like can occur, so that the physical and chemical properties of the catalyst material are obviously different from those of a regular bulk material, and the unique catalytic combustion performance is generated. A key issue in catalytic combustion technology is the development of high performance catalysts. In terms of economic cost, non-noble metal catalysts such as transition metal oxides are of great interest due to their low cost and low secondary pollution. There are two main catalysts for catalytic combustion of VOCs, which are noble metal and transition metal oxides. The transition metal oxide has good economic benefits and increases toxic by-products due to low cost, and the noble metal supported catalyst can have better catalytic activity and high selectivity at lower temperature. Document 1 (appl.surf.Sci.475 (2019) 312-324) reports that MnO is assembled in situ by taking Cr-MOF precursors as raw materials x As a high-stability toluene oxidation catalyst, the MnOx/Cr2O3 composite material prepared by pyrolysis shows good activity at 270 ℃, but the toluene as VOCs represents a single type and cannot be used as a real standard of mixed organic volatile gas discharged by engineering. Document 2 (Catal. Toady.375 (2021) 262.) reports Ag/Co prepared by solvothermal synthesis by a one-pot method 3 O 4 Catalyst for catalytic combustion of benzene 50％ And T 90％ The values are respectively as low as 181 ℃ and 201 ℃, but the temperature corresponding to 90% conversion rate is not ideal, and the treatment of low-concentration VOCs caused by home decoration and the treatment of low-concentration and low-energy-consumption VOCs in chemical plants cannot be realized. In the catalytic combustion reaction of VOCs, for example, in the case of any hydrocarbon substance, CO may be present in the produced product, and the binding capacity of CO and hemoglobin is stronger than that of oxygen, so that the long-term inhalation affects the health of human bodies. And another product CO 2 Is nontoxic, and can be widely used in carbonate, polyester fiber raw material, chemical processing, plant growth stimulant, and diluent of sterilizing gas. According to the practical application of the reaction product of the catalytic combustion of the VOCs and the current development situation of the low-temperature high-efficiency catalyst for catalytic combustion of the VOCs, a novel high-efficiency supported monatomic platinum MOFs-derived chromium-based catalyst with a simple synthesis method is developed, and the high-selectivity CO generation of low-concentration VOCs by high-efficiency low-temperature catalytic combustion is realized under mild conditions 2 Has very important scientific significance and application value.
Disclosure of Invention
In order to solve the problems, the invention provides a method for catalyzing and combusting solvent oil by using a MOFs-derived chromium-based catalyst loaded with monatomic platinum.
The technical scheme adopted by the invention is as follows:
a method for catalyzing and burning solvent oil by using a MOFs-derived chromium-based catalyst loaded with monatomic platinum comprises the steps of carrying out a solvent oil catalytic combustion reaction by using a tubular reactor, loading the MOFs-derived chromium-based catalyst loaded with monatomic platinum into the tubular reactor, mixing the solvent oil and air in a bubbling mode, blowing the mixture into the tubular reactor, controlling the flow of an inlet flow to be within 1.5L/min, and reacting at 120-240 ℃ for 2-24 hours; the concentration of VOCs is detected at the air inlet of the tubular reactor, and CO are detected at the air outlet 2 And the concentration of VOCs.
Further, the method for catalytic combustion of the solvent oil by using the above MOFs-derived chromium-based catalyst loaded with monatomic platinum is 100 # Or 150 # And (4) solvent oil.
Further, in the method for catalytic combustion of the solvent oil by using the above MOFs-derived chromium-based catalyst loaded with the monatomic platinum, the concentration of VOCs in the gas inlet is controlled to be 100-200ppm.
Further, the reaction temperature is 150-210 ℃, and the reaction time is 3-5 hours.
In the method for catalyzing and combusting the solvent oil by using the MOFs-derived chromium-based catalyst loaded with the monatomic platinum, the carrier is MIL-101 (Cr), and the metal platinum is dispersed on the carrier in an atomic level; the mass ratio of the carrier to the metal platinum is 28.3.
Furthermore, the preparation method of the above monatomic platinum-supported MOFs-derived chromium-based catalyst for catalytic combustion of the solvent oil comprises the following steps:
1) Uniformly mixing chromium nitrate nonahydrate, terephthalic acid, chloroplatinic acid aqueous solution, 20mL of deionized water and 0.2mL of 40% hydrofluoric acid solution, and transferring the mixture into a 100mL high-pressure reaction kettle lining;
2) Placing the high-pressure reaction kettle lining filled with the mixture in an ultrasonic washing device, carrying out ultrasonic treatment for 30min, and then transferring the high-pressure reaction kettle lining into a hydrothermal synthesis reaction kettle;
3) Placing the hydro-thermal synthesis reaction kettle in an air-blast drying oven at 220 ℃ for reacting for 8h, taking out and cooling to normal temperature;
4) And after the kettle is opened, transferring the dark green turbid liquid into a centrifugal tube for centrifugation, washing for 2-3 times by using deionized water, repeating the centrifugation process, placing the precipitate into a forced air drying oven at 80 ℃ for drying for 12 hours, taking out the precipitate, transferring the precipitate into a porcelain boat, and placing the porcelain boat into a muffle furnace for roasting.
Preferably, in the above preparation method of the monatomic platinum-supported MOFs-derived chromium-based catalyst, in step 1), the mass ratio of the chromium nitrate nonahydrate to the terephthalic acid is 2.5.
Preferably, in the preparation method of the above monatomic platinum-supported MOFs-derived chromium-based catalyst, in step 1), the preparation method of the chloroplatinic acid aqueous solution is: chloroplatinic acid was dispersed in water and sufficiently stirred to obtain a dispersion having a concentration of 0.01g/mL.
Preferably, in the above preparation method of the monatomic platinum supported MOFs-derived chromium-based catalyst, in step 4), the centrifugation condition is 12000rad/min for 3 minutes.
Preferably, in the preparation method of the above-mentioned monatomic platinum-supported MOFs-derived chromium-based catalyst, in step 4), the calcination is performed under the condition of calcination at 450 ℃ for 3 hours in an air atmosphere.
The beneficial effects of the invention are as follows:
1. the MOFs-derived chromium-based catalyst loaded with the monatomic platinum is prepared by a hydrothermal synthesis one-pot method, and the method has the advantages of simplicity in synthesis, simplicity in operation, environmental friendliness and the like, the platinum is dispersed on the carrier in an atomic level, the nano-sized particles with the size of 2-3nm are accumulated by observation of a transmission electron microscope, the catalyst has a high specific surface area, the catalyst has excellent catalytic activity in a 150# solvent naphtha catalytic combustion reaction, and a target product CO is generated with high selectivity 2 。
2. The MOFs-derived chromium-based catalyst loaded with monatomic platinum can realize a low-temperature high-selectivity reaction path, the solvent oil is catalyzed and combusted under the condition of no external oxygen supply, the catalysis temperature is reduced, the efficiency is high, and only CO is detected in the product 2 And nontoxic byproducts are generated, so that the method can be applied to the degradation of low-concentration VOCs in large-scale chemical plants.
3. The catalyst shows higher catalytic activity and stability at the optimal temperature point in the catalytic combustion reaction of low-concentration No. 150 solvent oil, the catalytic combustion efficiency at 150 ℃ is up to more than 94%, the catalytic combustion efficiency at 190 ℃ is up to 100%, no CO byproduct is generated in the process, and CO is generated 2 The selectivity is as high as 100%.
Drawings
FIG. 1 is a scanning electron micrograph of a MOFs-derived chromium-based catalyst supporting monatomic platinum.
Figure 2 is an XRD pattern of MOFs-derived chromium-based catalysts supporting monatomic platinum.
FIG. 3 is a MOFs-derived chromium-based catalyst catalytic combustion 150 at different temperatures with monatomic platinum loading # Graph of catalytic efficiency for mineral spirits.
FIG. 4 is a MOFs-derived chromium-based catalyst catalytic combustion 150 at different temperatures with monatomic platinum loading # CO in solvent oil reaction 2 Graph of concentration versus time.
Detailed Description
EXAMPLE 1 preparation of MOFs-derived chromium-based catalyst supporting monatomic platinum (Pt-MIL-101 (Cr))
1) Dispersing chromium nitrate nonahydrate, terephthalic acid and chloroplatinic acid in a mass ratio of 2.5 to 1 in an aqueous solution, fully stirring to obtain a dispersion (with the concentration of 0.01 g/mL), 20mL of deionized water and 0.2mL40% hydrofluoric acid solution measured by a liquid transfer gun, uniformly mixing, and transferring into a 100mL high-pressure reaction kettle lining;
2) Placing the lining of the high-pressure reaction kettle filled with the mixture in an ultrasonic washing device, carrying out ultrasonic treatment for 30min, and then transferring the lining into a hydrothermal synthesis reaction kettle;
3) Placing the hydro-thermal synthesis reaction kettle in an air-blowing drying box at 220 ℃ for reacting for 8 hours, taking out and cooling to normal temperature;
4) And after the kettle is opened, transferring the dark green suspension into a centrifugal tube for 3 minutes through 12000rad/min, washing the suspension with deionized water for 2-3 times, repeating the centrifugation process, placing the precipitate into a blast drying box at 80 ℃ for drying for 12 hours, taking the precipitate out, transferring the precipitate into a porcelain boat, placing the porcelain boat into a muffle furnace, and roasting the porcelain boat for 3 hours at 450 ℃ in an air atmosphere to obtain the monatomic platinum-loaded MOFs-derived chromium-based catalyst (Pt-MIL-101 (Cr)).
A small amount of the prepared MOFs-derived chromium-based catalyst loaded with monatomic platinum is dispersed in ethanol, the dispersed sample is dropped on a copper mesh after ultrasonic treatment for 10min to carry out scanning electron microscope test, and the scanning result is shown in figure 1, so that the small particle size and the good dispersibility can be clearly observed.
A small amount of prepared MOFs-derived chromium-based catalyst loaded with monatomic platinum is taken to carry out XRD test, the test result is shown in figure 2, the wide peak width indicates that the particle size of the sample is small, the crystallinity is general, and therefore, the catalyst has a high specific surface area and excellent catalytic performance.
Example 2 method for catalytic combustion of mineral spirit by using MOFs derived chromium based catalyst loaded with monatomic platinum
Adopting a tubular reactor to carry out catalytic combustion reaction of solvent oil, accurately weighing 0.5g of MOFs-derived chromium-based catalyst loaded with monatomic platinum, and placing the catalyst in a straight glass tube for reactionIn the reactor, quartz wool is attached to two ends of the catalyst to prevent catalyst powder from entering the pipeline along with the air flow, and 150 is bubbled # Solvent oil and air are mixed and blown into the tubular reactor, the inlet flow rate is controlled within 1.5L/min, a handheld VOCs detector is adopted to detect the concentration of VOCs at an air inlet before the reaction starts, the concentration of the inlet VOCs is controlled between 100 ppm and 200ppm, the catalytic combustion reaction is started after the concentration of the air inlet is stable, the reaction is carried out for 2 to 24 hours at 120 ℃ to 240 ℃, the gas concentration at an air outlet is detected after the temperature point is reached and stabilized for 10 minutes, and the detection is carried out for more than 15 minutes after the gas concentration is stabilized. CO and CO detected by gas outlet 2 The catalytic efficiency was calculated from the concentration of VOCs and the detailed results are shown in table 1.
TABLE 1 catalytic Combustion reaction results
FIG. 3 makes it possible to see T of the activity of the MOFs-derived chromium-based catalysts supporting monatomic platinum 90％ The point is 150-180 ℃, and the low-temperature high-activity performance is shown.
FIG. 4 shows that the higher the temperature the higher the CO 2 The time to reach equilibrium is shortened, CO 2 The content is increased, and in addition, no byproducts such as CO and the like are generated in the process.
Claims (10)
1. A method for catalytic combustion of solvent oil by using a monatomic platinum-loaded MOFs-derived chromium-based catalyst is characterized in that a tubular reactor is adopted for catalytic combustion reaction of the solvent oil, the monatomic platinum-loaded MOFs-derived chromium-based catalyst is loaded into the tubular reactor, the solvent oil and air are mixed and blown into the tubular reactor in a bubbling mode, the inlet flow is controlled within 1.5L/min, and the reaction is carried out for 2-24 hours at 120-240 ℃; the concentration of VOCs is detected at the air inlet of the tubular reactor, and CO are detected at the air outlet 2 And the concentration of VOCs.
2. The method for catalytic combustion of mineral spirits by using monatomic platinum-supported MOFs-derived chromium-based catalyst according to claim 1, wherein said mineral spirits is obtained by using said catalystIs 100 # Or 150 # Solvent oil.
3. The method for catalytic combustion of mineral spirits by using a MOFs-derived chromium-based catalyst loaded with monatomic platinum according to claim 1, wherein the concentration of VOCs in said gas inlet is controlled to be 100-200ppm.
4. The method for catalytic combustion of mineral spirits of the MOFs-derived chromium-based catalyst carrying monatomic platinum according to claim 1, wherein said reaction temperature is 150 ℃ to 210 ℃ and the reaction time is 3 to 5 hours.
5. The method for catalytic combustion of mineral spirits by MOFs-derived chromium-based catalyst loaded with monatomic platinum according to any of claims 1 to 4, characterized in that said monatomic platinum loaded MOFs-derived chromium-based catalyst is MIL-101 (Cr) and the metallic platinum is dispersed on the carrier at atomic level; the mass ratio of the carrier to the metal platinum is 28.3.
6. The method for catalytic combustion of mineral spirits by a monatomic platinum-loaded MOFs-derived chromium-based catalyst according to claim 5, characterized in that the preparation method of said monatomic platinum-loaded MOFs-derived chromium-based catalyst comprises the following steps:
1) Uniformly mixing chromium nitrate nonahydrate, terephthalic acid, chloroplatinic acid aqueous solution, 20mL of deionized water and 0.2mL of 40% hydrofluoric acid solution, and transferring the mixture into a 100mL high-pressure reaction kettle lining;
2) Placing the lining of the high-pressure reaction kettle filled with the mixture in an ultrasonic washing device, carrying out ultrasonic treatment for 30min, and then transferring the lining into a hydrothermal synthesis reaction kettle;
3) Placing the hydro-thermal synthesis reaction kettle in an air-blast drying oven at 220 ℃ for reacting for 8h, taking out and cooling to normal temperature;
4) And after the kettle is opened, transferring the dark green turbid liquid into a centrifugal tube for centrifugation, washing for 2-3 times by using deionized water, repeating the centrifugation process, placing the precipitate into a forced air drying oven at 80 ℃ for drying for 12 hours, taking out the precipitate, transferring the precipitate into a porcelain boat, and placing the porcelain boat into a muffle furnace for roasting.
7. The method for catalytic combustion of mineral spirits of the MOFs-derived chromium-based catalyst carrying monatomic platinum according to claim 6, wherein in the step 1), the mass ratio of said chromium nitrate nonahydrate to said terephthalic acid is 2.5.
8. The method for catalytic combustion of the solvent oil by using the MOFs-derived chromium-based catalysts loaded with the monatomic platinum according to claim 6, wherein in the step 1), the preparation method of the chloroplatinic acid aqueous solution comprises the following steps: chloroplatinic acid was dispersed in water and sufficiently stirred to obtain a dispersion having a concentration of 0.01g/mL.
9. The method for catalytic combustion of mineral spirits of a catalyst based on MOFs derived chromium carrying monatomic platinum according to claim 6, wherein in step 4) said centrifugation conditions are 12000rad/min for 3 minutes.
10. The method for catalytic combustion of mineral spirits of the MOFs-derived chromium-based catalyst carrying monatomic platinum according to claim 6, wherein in the step 4), the calcination condition is 450 ℃ for 3 hours in an air atmosphere.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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