CN114870855B - Metal catalyst compound and preparation method thereof - Google Patents
Metal catalyst compound and preparation method thereof Download PDFInfo
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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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01D53/34—Chemical or biological purification of waste gases
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Abstract
The invention provides a metal catalyst compound, the carrier of the catalyst is modified gamma-Al 2 O 3 The active components are manganese-containing metal salt, cerium-containing metal salt, copper-containing metal salt and yttrium-containing metal salt; the modified gamma-Al 2 O 3 The preparation method of (2) comprises the following steps: gamma-Al 2 O 3 Immersing in nitric acid, adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid, stirring, standing to form gel, constant-temp extruding to obtain particles, and carbonizing to obtain modified gamma-Al 2 O 3 . The invention adds lanthanum nitrate and chlorinated paraffin to gamma-Al 2 O 3 The high temperature resistance of the metal catalyst compound is effectively improved by modifying, and the phenomenon of high temperature sintering in the use process of the catalyst is avoided.
Description
Technical Field
The invention relates to the technical field of metal catalysts, in particular to a metal catalyst compound and a preparation method thereof.
Background
With the rapid development of modern industry in China, the content of volatile organic compounds (VoCs) in the atmosphere is gradually increased, and the VoCs are generated and discharged into the atmosphere in the production and use processes of petrochemical industry, printing, paint, coating and the like. VOCs in the air can destroy the ozone layer, cause acid rain and generate photochemical smog, and directly harm human health. The treatment methods of VOCs generally include an absorption method, a biological method, a condensation method and the like, and the catalytic oxidation method is widely focused on the advantages of wide application range, low ignition temperature, high treatment efficiency, low secondary pollution and the like for treating VOCs waste gas with low concentration and no recycling value. At present, the catalytic oxidation VOCs catalyst mainly comprises three types of noble metal, non-noble metal and molecular sieve catalyst, the noble metal catalyst mainly uses noble metals such as Pt, pd, rh and the like as active components, and is widely applied to the catalytic industry, and has the characteristics of low-temperature light-off property, high catalytic oxidation activity and the like, but the problems of high-temperature sintering and low catalytic efficiency are easy to occur in the actual application process.
Disclosure of Invention
In view of the above, the invention provides a metal catalyst compound with high catalytic efficiency and low probability of high-temperature sintering and a preparation method thereof.
The technical scheme of the invention is realized as follows: in one aspect, the invention provides a metal catalyst composite, the carrier of the catalyst is modified gamma-Al 2 O 3 The active components are manganese-containing metal salt, cerium-containing metal salt, copper-containing metal salt and yttrium-containing metal salt; the modified gamma-Al 2 O 3 The preparation method of (2) comprises the following steps: gamma-Al 2 O 3 Immersing in nitric acid, adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid, stirring, standing to form gel, constant-temp extruding to obtain particles, and carbonizing to obtain modified gamma-Al 2 O 3 。
On the basis of the technical scheme, preferably, the gamma-Al 2 O 3 The mass ratio of lanthanum nitrate to chlorinated paraffin to cellulose to citric acid is (10-15), (2-5), (1-3), (3-5) and (2-3).
Based on the technical scheme, the constant-temperature extrusion temperature is preferably 130-150 ℃, the pressure is 10-20MPa, and the carbonization temperature is 300-700 ℃.
On the basis of the technical scheme, preferably, the gamma-Al 2 O 3 The mass concentration in nitric acid is 10-15%.
On the basis of the technical scheme, preferably, the manganese-containing metal salt, the cerium-containing metal salt, the copper-containing metal salt and the yttrium-containing metal salt are all selected from nitrate.
In another aspect, the present invention provides a method of preparing a metal catalyst composite, comprising the steps of: dissolving manganese-containing metal salt, cerium-containing metal salt, copper-containing metal salt and yttrium-containing metal salt in isopropanol, and adding modified gamma-Al 2 O 3 Reacting at 150-200deg.C for 4-6h, cooling to 20-30deg.C, centrifuging to separate solid, washing the solid with deionized water,until the washing liquid is neutral, the solid is dried and calcined to obtain the metal catalyst compound.
On the basis of the technical proposal, preferably, the manganese-containing metal salt is cerium-containing metal salt, copper-containing metal salt, yttrium-containing metal salt and gamma-Al 2 O 3 The mass ratio of (5-7): (3-5): (2-3): (0.5-1): (2-5).
On the basis of the technical scheme, preferably, the calcination conditions are as follows: calcining at 400-700 deg.c for 3-5 hr in nitrogen atmosphere, converting to air atmosphere, calcining for 2-3 hr, and cooling naturally.
On the basis of the technical scheme, the metal catalyst compound is preferably used for oxidation catalysis of the diisocyanatotoluene ester.
Compared with the prior art, the metal catalyst compound and the preparation method thereof have the following beneficial effects: the invention adds lanthanum nitrate and chlorinated paraffin to gamma-Al 2 O 3 The high temperature resistance of the metal catalyst compound is effectively improved by modifying, and the phenomenon of high temperature sintering in the use process of the catalyst is avoided. Wherein, the addition of chlorinated paraffin can increase gamma-Al 2 O 3 Internal channel, increase gamma-Al 2 O 3 And increase the porosity of gamma-Al 2 O 3 Is a compound having an activity of (a); lanthanum nitrate can inhibit gamma-Al on the basis 2 O 3 High-temperature sintering collapse, and the specific surface area and the pore diameter are reduced; lanthanum nitrate and chlorinated paraffin act synergistically to increase the high temperature resistance of the metal catalyst.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph of the catalytic performance of the metal catalyst composite of the present invention for diisocyanatotoluene esters;
FIG. 2 is a graph of the performance of the comparative example in catalyzing diisocyanatotoluene.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Example 1
The metal catalyst composite of the embodiment, the carrier of the catalyst is modified gamma-Al 2 O 3 The active components are manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate.
Modified gamma-Al 2 O 3 The preparation method of (2) comprises the following steps: gamma-Al 2 O 3 Immersing in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid is 10%; adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to a certain proportion, stirring uniformly, standing for 1h to form gel, extruding at 130 ℃ and 10MPa at constant temperature to form particles, and carbonizing at 300 ℃ to obtain modified gamma-Al 2 O 3 . Wherein gamma-Al 2 O 3 The mass ratio of lanthanum nitrate to chlorinated paraffin to cellulose to citric acid is 10:2:1:3:2.
A method of preparing a metal catalyst composite comprising the steps of: sequentially dissolving manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate in isopropanol, and adding modified gamma-Al 2 O 3 Reacting for 4 hours at 150 ℃, cooling to 20 ℃, centrifugally separating out solid, washing the solid by adopting deionized water until the washing liquid is neutral, drying the solid for 2 hours at 80 ℃, and calcining to obtain the metal catalyst compound. The calcination conditions are as follows: calcining for 3h at 400 ℃ in nitrogen atmosphere, converting into air atmosphere, continuously calcining for 2h, and naturally cooling. Manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate, yttrium nitrate hexahydrate and gamma-Al 2 O 3 The mass ratio of (2) is 5:3:2:0.5:2.
Example two
The metal catalyst composite of the embodiment, the carrier of the catalyst is modified gamma-Al 2 O 3 The active components are manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate.
Modified gamma-Al 2 O 3 The preparation method of (2) comprises the following steps: gamma-Al 2 O 3 Immersing in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid is 12%; adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to a certain proportion, stirring uniformly, standing for 1.5h to form gel, extruding at constant temperature of 140 ℃ and 15MPa to form particles, and carbonizing at 300 ℃ to obtain modified gamma-Al 2 O 3 。γ-Al 2 O 3 The mass ratio of lanthanum nitrate to chlorinated paraffin to cellulose to citric acid is 11:3:1.5:4:2.5.
A method of preparing a metal catalyst composite comprising the steps of: sequentially dissolving manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate in isopropanol, and adding modified gamma-Al 2 O 3 Reacting at 160 ℃ for 4.5 hours, cooling to 25 ℃, centrifugally separating out solid, washing the solid by adopting deionized water until the washing liquid is neutral, drying the solid at 80 ℃ for 2 hours, and calcining to obtain the metal catalyst compound. The calcination conditions are as follows: calcining for 4 hours at 500 ℃ under nitrogen atmosphere, then converting into air atmosphere, continuously calcining for 2.5 hours, and naturally cooling. Manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate, yttrium nitrate hexahydrate and gamma-Al 2 O 3 The mass ratio of (2) is 6:4:2.5:0.6:3.
Example III
The metal catalyst composite of the embodiment, the carrier of the catalyst is modified gamma-Al 2 O 3 The active components are manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate.
Modified gamma-Al 2 O 3 The preparation method of (2) comprises the following steps: gamma-Al 2 O 3 Immersing in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid was 14%; then adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to the proportionStirring uniformly, standing for 2h to form gel, extruding at 145 ℃ and 15MPa to form particles, and carbonizing at 500 ℃ to obtain modified gamma-Al 2 O 3 。γ-Al 2 O 3 The mass ratio of lanthanum nitrate to chlorinated paraffin to cellulose to citric acid is 13:4:2:4.5:3.
A method of preparing a metal catalyst composite comprising the steps of: sequentially dissolving manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate in isopropanol, and adding modified gamma-Al 2 O 3 Reacting at 180 ℃ for 5 hours, cooling to 25 ℃, centrifugally separating out solid, washing the solid by adopting deionized water until the washing liquid is neutral, drying the solid at 80 ℃ for 2 hours, and calcining to obtain the metal catalyst compound. The calcination conditions are as follows: calcining at 600 ℃ for 4 hours under nitrogen atmosphere, then converting into air atmosphere, continuously calcining for 3 hours, and naturally cooling. Manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate, yttrium nitrate hexahydrate and gamma-Al 2 O 3 The mass ratio of (2) is 7:5:3:1:4.
Example IV
The metal catalyst composite of the embodiment, the carrier of the catalyst is modified gamma-Al 2 O 3 The active components are manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate.
Modified gamma-Al 2 O 3 The preparation method of (2) comprises the following steps: gamma-Al 2 O 3 Immersing in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid is 15%; adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to a certain proportion, stirring uniformly, standing for 2h to form gel, extruding at constant temperature of 150 ℃ and 20MPa to form particles, and carbonizing at 700 ℃ to obtain modified gamma-Al 2 O 3 。γ-Al 2 O 3 The mass ratio of lanthanum nitrate to chlorinated paraffin to cellulose to citric acid is 15:5:3:5:3.
A method of preparing a metal catalyst composite comprising the steps of: sequentially dissolving manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate in isopropanol, and adding modified gamma-Al 2 O 3 Reacting for 6h at 200 DEG CCooling to 30 ℃, centrifugally separating out solid, washing the solid by adopting deionized water until the washing liquid is neutral, drying the solid at 80 ℃ for 2 hours, and calcining to obtain the metal catalyst compound. The calcination conditions are as follows: calcining at 700 ℃ for 5h under nitrogen atmosphere, converting into air atmosphere, continuously calcining for 3h, and naturally cooling. Manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate, yttrium nitrate hexahydrate and gamma-Al 2 O 3 The mass ratio of (2) is 7:5:3:1:5.
Comparative example one
Comparative example one example was followed, except that the catalyst support was gamma-Al 2 O 3 。
Comparative example two
Comparative example two differs from example one in that gamma-Al was modified 2 O 3 The preparation process of (2) lacks chlorinated paraffin.
Comparative example three
Comparative example III As example one, the difference is that gamma-Al was modified 2 O 3 Lanthanum nitrate is absent from the preparation process.
Comparative example four
Comparative example four is the same as example one except that the active ingredient does not contain yttrium metal salt.
Catalytic oxidation performance test:
the metal catalyst composites prepared in examples and comparative examples were ground to 30 mesh and placed in a scanning plasma apparatus. The test conditions were: the total flow rate of the gas was 100ml/min, the concentration of the diisocyanatotoluene ester was 30ppm, the carrier was dry air, and the concentration of the diisocyanatotoluene ester was detected by gas chromatography, and the result is shown in FIG. 1:
1-2, the catalytic capacities of the metal catalyst composites of examples 1-4 of the present invention are much higher than those of comparative examples 1-4; modified gamma-Al 2 O 3 When the preparation method lacks chlorinated paraffin or lanthanum nitrate, the catalytic efficiency of the catalyst at high temperature is obviously reduced; the catalytic efficiency was also reduced relative to examples 1-4 when the active component did not contain yttrium metal salt.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. A method for preparing a metal catalyst composite, characterized by: the carrier of the catalyst is modified gamma-Al 2 O 3 The active components are manganese-containing metal salt, cerium-containing metal salt, copper-containing metal salt and yttrium-containing metal salt; the modified gamma-Al 2 O 3 The preparation method of (2) comprises the following steps: gamma-Al 2 O 3 Immersing in nitric acid, adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid, stirring, standing to form gel, constant-temp extruding to obtain particles, and carbonizing to obtain modified gamma-Al 2 O 3 ；
The preparation method of the metal catalyst composite comprises the following steps: dissolving manganese-containing metal salt, cerium-containing metal salt, copper-containing metal salt and yttrium-containing metal salt in isopropanol, and adding modified gamma-Al 2 O 3 Reacting for 4-6h at 150-200 ℃, cooling to 20-30 ℃, centrifuging to separate out solid, washing the solid with deionized water until the washing liquid is neutral, and drying and calcining the solid to obtain the metal catalyst compound.
2. A method of preparing a metal catalyst composite according to claim 1, wherein: the gamma-Al 2 O 3 The mass ratio of lanthanum nitrate to chlorinated paraffin to cellulose to citric acid is (10-15), (2-5), (1-3), (3-5) and (2-3).
3. A method of preparing a metal catalyst composite according to claim 1, wherein: the constant-temperature extrusion temperature is 130-150 ℃, the pressure is 10-20MPa, and the carbonization temperature is 300-700 ℃.
4. A method of preparing a metal catalyst composite according to claim 1, wherein: the gamma-Al 2 O 3 The mass concentration in nitric acid is 10-15%.
5. A method of preparing a metal catalyst composite according to claim 1, wherein: the manganese-containing metal salt, cerium-containing metal salt, copper-containing metal salt and yttrium-containing metal salt are all selected from nitrates.
6. A method of preparing a metal catalyst composite according to claim 1, wherein: the manganese-containing metal salt is cerium-containing metal salt, copper-containing metal salt, yttrium-containing metal salt and gamma-Al 2 O 3 The mass ratio of (5-7): (3-5): (2-3): (0.5-1): (2-5).
7. A method of preparing a metal catalyst composite according to claim 1, wherein: the calcination conditions are as follows: calcining at 400-700 deg.c for 3-5 hr in nitrogen atmosphere, converting to air atmosphere, calcining for 2-3 hr, and cooling naturally.
8. A method of preparing a metal catalyst composite according to claim 1, wherein: the metal catalyst composite is used for oxidizing and catalyzing the diisocyanatotoluene ester.
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