CN114870855A - Metal catalyst compound and preparation method thereof - Google Patents
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Abstract
The invention provides a metal catalyst compound, wherein 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 comprises the following steps: mixing gamma-Al 2 O 3 Immersing in nitric acid, adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid, stirring, standing to form gel, extruding at constant temperature to obtain granules, and carbonizing to obtain modified gamma-Al 2 O 3 . The invention adds lanthanum nitrate and chloroparaffin para-gamma-Al 2 O 3 The modification effectively improves the high temperature resistance of the metal catalyst compound and avoids the high temperature sintering phenomenon in the use process of the catalyst.
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, which are generated and discharged into the atmosphere in the production and use processes of petrochemical industry, printing, paints, coatings 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 method of the VOCs generally comprises an absorption method, a biological method, a condensation method and the like, and the catalytic oxidation method has wide attention due to the advantages of wide application range, low ignition temperature, high treatment efficiency, small secondary pollution and the like for treating the VOCs waste gas with low concentration and no recycling value. At present, the catalytic oxidation VOCs catalyst mainly comprises three types of noble metals, non-noble metals and molecular sieve catalysts, the noble metal catalyst mainly takes noble metals such as Pt, Pd, Rh and the like as active components, the noble metal catalyst is widely applied to the catalysis industry, and has the characteristics of low-temperature ignition performance, high catalytic oxidation activity and the like, but the problems of high-temperature sintering and low catalytic efficiency are easy to occur in the practical application process.
Disclosure of Invention
In view of the above, the invention provides a metal catalyst composite with high catalytic efficiency and difficult high-temperature sintering and a preparation method thereof.
The technical scheme of the invention is realized as follows: in one aspect, the present invention provides a metal catalyst composite, wherein 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 comprises the following steps: mixing gamma-Al 2 O 3 Immersing in nitric acid, adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid, stirring, standing to form gel, extruding at constant temperature to obtain granules, and carbonizing to obtain modified gamma-Al 2 O 3 。
Based on the above technical solution, preferably, the γ -Al 2 O 3 The mass ratio of lanthanum nitrate, chlorinated paraffin, cellulose and citric acid is (10-15): (2-5): 1-3): 3-5): 2-3.
On the basis of the technical scheme, preferably, the temperature of the constant-temperature extrusion is 130-150 ℃, the pressure is 10-20MPa, and the carbonization temperature is 300-700 ℃.
Based on the above technical solution, preferably, the γ -Al 2 O 3 The mass concentration in nitric acid is 10-15%.
Based on the above technical solution, 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 nitrates.
In another aspect, the present invention provides a method for 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 for 4-6h at the temperature of 150-200 ℃, then cooling to 20-30 ℃, centrifugally separating out solid, washing the solid by deionized water until the washing liquid is neutral, and drying and calcining the solid to obtain the metal catalyst compound.
Based on the above technical scheme, 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) to (3-5) to (2-3) to (0.5-1) to (2-5).
On the basis of the above technical solution, preferably, the calcination conditions are: calcining for 3-5h at the temperature of 400-700 ℃ under the nitrogen atmosphere, then converting into the air atmosphere to continue calcining for 2-3h, and naturally cooling.
On the basis of the technical scheme, preferably, the metal catalyst compound is used for oxidizing and catalyzing diisotolyl diisocyanate.
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 chloroparaffin para-gamma-Al 2 O 3 The modification effectively improves the high temperature resistance of the metal catalyst compound and avoids the high temperature sintering phenomenon in the use process of the catalyst. Wherein the chlorinated paraffin can be added with gamma-Al 2 O 3 Internal passages, adding gamma-Al 2 O 3 Porosity of, increasing gamma-Al 2 O 3 Activity of (a); on the basis, lanthanum nitrate can inhibit gamma-Al 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, so that the high temperature resistance of the metal catalyst is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph showing the performance of the metal catalyst composite of the present invention in catalyzing diisocyanatophenyl ester;
FIG. 2 is a graph showing the performance of a comparative example for catalyzing a toluene diisocynate.
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 obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example one
The metal catalyst composite of this example, the carrier of the catalyst was modified γ -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 comprises the following steps: mixing gamma-Al 2 O 3 Immersing in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid is 10 percent; then adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to a proportion, stirring uniformly, standing for 1h to form gel, extruding into granules at a constant temperature of 130 ℃ and under 10MPa, and carbonizing at 300 ℃ to obtain the 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 for preparing a metal catalyst composite comprisingThe method comprises the following steps: 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 150 ℃ for 4h, cooling to 20 ℃, centrifugally separating out solid, washing the solid by deionized water until the washing liquid is neutral, drying the solid at 80 ℃ for 2h, and calcining to obtain the metal catalyst composite. The calcination conditions were: calcining at 400 ℃ for 3h in nitrogen atmosphere, then converting into air atmosphere to continue 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 (A) to (B) is 5:3:2:0.5: 2.
Example two
The metal catalyst composite of this example, the carrier of the catalyst was modified γ -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 comprises the following steps: gamma-Al is mixed 2 O 3 Immersion in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid is 12 percent; then adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to a proportion, stirring uniformly, standing for 1.5h to form gel, extruding into granules at a constant temperature of 140 ℃ and 15MPa, and carbonizing at 300 ℃ to obtain the 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 for 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 4.5h, cooling to 25 ℃, centrifugally separating out solid, washing the solid by deionized water until the washing liquid is neutral, drying the solid at 80 ℃ for 2h, and calcining to obtain the metal catalyst compound. The calcination conditions were: calcining at 500 deg.C for 4h in nitrogen atmosphere, then converting to air atmosphere, calcining for 2.5h, and naturally cooling. Manganese nitrate tetrahydrate, cerium nitrate hexahydrate, copper nitrate and yttrium nitrate hexahydrate:γ-Al 2 O 3 The mass ratio of (A) to (B) 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 comprises the following steps: mixing gamma-Al 2 O 3 Immersion in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid is 14 percent; then adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to a proportion, stirring uniformly, standing for 2h to form gel, extruding into granules at a constant temperature of 145 ℃ and 15MPa, and carbonizing at 500 ℃ to obtain the 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 for 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 5h, cooling to 25 ℃, centrifugally separating out solid, washing the solid by deionized water until the washing liquid is neutral, drying the solid at 80 ℃ for 2h, and calcining to obtain the metal catalyst compound. The calcination conditions were: calcining at 600 ℃ for 4h in nitrogen atmosphere, then converting into air atmosphere to continue 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 (1) to (2) is 7:5:3:1: 4.
Example four
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 comprises the following steps: mixing gamma-Al 2 O 3 Immersion in nitric acid, gamma-Al 2 O 3 The mass concentration in nitric acid is 15 percent; however, the device is not suitable for use in a kitchenThen adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid according to a proportion, stirring uniformly, standing for 2h to form gel, extruding into granules at a constant temperature of 150 ℃ and 20MPa, and carbonizing at 700 ℃ to obtain the modified gamma-Al 2 O 3 。γ-Al 2 O 3 The mass ratio of the lanthanum nitrate to the chlorinated paraffin to the cellulose to the citric acid is 15:5:3:5: 3.
A method for 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 200 ℃ for 6h, cooling to 30 ℃, centrifugally separating out solid, washing the solid by deionized water until the washing liquid is neutral, drying the solid at 80 ℃ for 2h, and calcining to obtain the metal catalyst compound. The calcination conditions were: calcining at 700 deg.C for 5h in nitrogen atmosphere, converting into air atmosphere, 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 (1) to (2) is 7:5:3:1: 5.
Comparative example 1
Comparative example one is identical except that the catalyst support is γ -Al 2 O 3 。
Comparative example No. two
Comparative example two the same as example one except for the modified gamma-Al 2 O 3 The preparation method of (1) lacks chlorinated paraffin.
Comparative example No. three
Comparative example three examples are the same as example one except that gamma-Al is modified 2 O 3 The preparation method of (1) lacks lanthanum nitrate.
Comparative example No. four
Comparative example four the same as example one except that the active component does not contain yttrium metal salt.
And (3) testing catalytic oxidation performance:
the metal catalyst composites prepared in examples and comparative examples were put into a scanning plasma apparatus by grinding to 30 mesh. The test conditions were: the total gas flow was 100ml/min, the diisocyanatotoluene concentration was 30ppm, the carrier was dry air, the diisocyanatobenzene ester concentration was determined by gas chromatography, and the results are shown in fig. 1:
as shown in fig. 1-2, the metal catalyst composites of examples 1-4 of the present invention have much higher catalytic abilities than those of comparative examples 1-4; modified gamma-Al 2 O 3 When the preparation method of (2) lacks chlorinated paraffin or lanthanum nitrate, the catalytic efficiency of the catalyst at high temperature is obviously reduced; the catalytic efficiency is also reduced relative to examples 1-4 when the active component does not contain yttrium metal salt.
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 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 comprises the following steps: mixing gamma-Al 2 O 3 Immersing in nitric acid, adding lanthanum nitrate, chlorinated paraffin, cellulose and citric acid, stirring, standing to form gel, extruding at constant temperature to obtain granules, and carbonizing to obtain modified gamma-Al 2 O 3 。
2. A metal catalyst composite according to claim 1, wherein: the gamma-Al 2 O 3 The mass ratio of lanthanum nitrate, chlorinated paraffin, cellulose and citric acid is (10-15): (2-5): 1-3): 3-5): 2-3.
3. A metal catalyst composite according to claim 1, wherein: the temperature of the constant-temperature extrusion is 130-150 ℃, the pressure is 10-20MPa, and the carbonization temperature is 300-700 ℃.
4. A metal catalyst composite according to claim 1, wherein: the gamma is-Al 2 O 3 The mass concentration in nitric acid is 10-15%.
5. A metal catalyst composite according to claim 1, wherein: the manganese-containing metal salt, the cerium-containing metal salt, the copper-containing metal salt and the yttrium-containing metal salt are selected from nitrates.
6. The method of claim 1, wherein the metal catalyst composite is prepared by: the method 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 the temperature of 150-200 ℃, then cooling to 20-30 ℃, centrifugally separating out solid, washing the solid by deionized water until the washing liquid is neutral, and drying and calcining the solid to obtain the metal catalyst compound.
7. The method of claim 6, wherein the metal catalyst composite is prepared by: 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) to (3-5) to (2-3) to (0.5-1) to (2-5).
8. The method of claim 6, wherein the metal catalyst composite is prepared by: the calcination conditions are as follows: calcining for 3-5h at the temperature of 400-700 ℃ under the nitrogen atmosphere, then converting into the air atmosphere to continue calcining for 2-3h, and naturally cooling.
9. A metal catalyst composite according to claim 1, wherein: the metal catalyst compound is used for oxidizing and catalyzing diisotolyl diisocyanate.
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