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Self-supporting palladium-based catalyst as well as preparation method and application thereof

A catalyst, self-supporting technology, applied in catalyst activation/preparation, carbon monoxide or formate reaction preparation, chemical instruments and methods, etc., can solve the problem of high loading of precious metal Pd, catalyst bed "hot spots, and difficulty in reactor heat transfer" and other problems, to achieve the effect of controllable structure, easy molding, good mass and heat transfer performance

Pending Publication Date: 2018-12-14
ECO ENVIRONMENTAL ENERGY RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the low thermal conductivity of the reported catalyst system will inevitably lead to difficulty in heat removal in the reactor, easy to cause "hot spots" in the catalyst bed and even runaway temperature control, which will not only cause catalytic and non-catalytic degradation of nitrite raw materials. Decomposition will reduce the selectivity, and will lead to catalyst sintering deactivation and even safety accidents
In addition, the noble metal Pd loading of the currently reported catalysts is high, and the catalysts are expensive.

Method used

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  • Self-supporting palladium-based catalyst as well as preparation method and application thereof
  • Self-supporting palladium-based catalyst as well as preparation method and application thereof
  • Self-supporting palladium-based catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] ① Weigh 4 grams of aluminum fiber (fiber diameter 80 microns, length 4-10 mm), soak it in 1.0 wt% sodium hydroxide aqueous solution at room temperature for 3-10 minutes, wash with distilled water and transfer to 100 ml Stainless steel autoclave, add distilled water until the aluminum fibers are completely submerged, seal the autoclave and place it in an oven for static hydrothermal treatment at 120°C for 24 hours, wash with distilled water and dry to obtain aluminum fiber-porous pseudoboehmite composite carrier;

[0059] 2. Dissolve 0.0260 g of palladium acetate in acetone solution, then weigh 0.1109 g of 3-aminopropyltriethoxysilane and add it to the palladium acetate in acetone solution; weigh step 1. Gained aluminum fiber-porous pseudoboehmite composite carrier 4 gram, was added to the palladium acetate acetone solution complexed by 3-aminopropyltriethoxysilane, dried after equal volume impregnation at room temperature; said 0.1032 g of sodium nitrate was dissolved i...

Embodiment 2

[0070] 1. with step 1. in embodiment 1;

[0071] 2. With the acetone solution containing 0.0260 gram of palladium acetate, impregnate 4 grams of step 1. Gained aluminum fiber-porous pseudo-boehmite composite carrier, after drying, place in high-purity N 2 Pyrolysis treatment at 350°C under protection for 1 hour, cooling to room temperature and taking out, the self-supporting carbon-modified metal palladium catalyst of the present invention was obtained, and the mass contents of Pd and C were respectively 0.26% and 0.1% by elemental quantitative analysis. %, recorded as 0.26Pd-0.1C / Al80-fiber.

[0072] Figure 4 , Figure 5 with Image 6 X-ray diffraction spectrum, scanning electron microscope (SEM) and transmission electron microscope (TEM) of the self-supporting carbon-modified metal palladium catalyst 0.26Pd-0.1C / Al80-fiber prepared for this example. Depend on Figure 4 It can be seen that in addition to the diffraction peak of aluminum fiber, the diffraction peak of ps...

Embodiment 3

[0075] 1. Weigh 10 grams of aluminum fiber felt (fiber diameter 60 microns), soak it in 2.0 wt% sodium hydroxide aqueous solution at room temperature for 3 to 10 minutes, wash it with distilled water and transfer it to a 100 ml stainless steel autoclave, add Distill water until the aluminum tube is completely submerged, seal the kettle and place it in an oven for static hydrothermal treatment at 120°C for 2 hours, wash with distilled water and dry to obtain the aluminum fiber felt-porous pseudo-boehmite composite carrier;

[0076] 2. With the acetone solution containing 0.026 gram of palladium acetate, impregnate 4 grams of aluminum fiber mat-porous pseudo-boehmite composite carrier obtained in step 1. After drying, place in high-purity N 2 Pyrolysis treatment at 350°C under protection for 1 hour, cooling to room temperature and taking out, the self-supporting carbon-modified metal palladium catalyst of the present invention was obtained, and the mass content of Pd and C were r...

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Abstract

The invention discloses a self-supporting carbon or carbon-oxide or carbon-nitrogen-oxide modified metal palladium catalyst as well as a preparation method and application thereof. The self-supportingpalladium-based catalyst is a carbon or carbon-oxide or carbon-nitrogen-oxide modified metal palladium catalyst loaded on a porous oxide-anchoring carrier. The catalyst is prepared by the steps thata carrier is subjected to porous treatment through acid or alkali and hydrothermal treatment or through acid or alkali or hydrothermal treatment and then roasted, and thus the porous oxide-anchoring carrier is prepared; and then the prepared porous surface carrier is subjected to isometric impregnation and pyrolysis treatment through a solution containing one or more of a palladium precursor, a carbon precursor, a nitrogen precursor and an oxide precursor, and thus the self-supporting palladium-based catalyst is prepared. The self-supporting palladium-based catalyst can be used for reaction ofsynthesizing dimethyl carbonate through carbon monoxide and nitrous acid ester, reaction of synthesizing methyl formate by formylating methyl nitrite through carbon monoxide, and reaction of synthesizing dimethyl oxalate through carbon monoxide and nitrous acid ester.

Description

technical field [0001] The invention relates to a self-supporting palladium-based catalyst and its preparation method and application, in particular, to a porous anchored oxide carrier loaded with carbon or carbon-oxide or carbon-nitrogen-oxide modification Metal palladium catalyst and preparation method thereof, and carbon monoxide and methyl nitrite in the reaction of carbon monoxide and nitrite to synthesize dimethyl carbonate, carbon monoxide and methyl nitrite carry out methyl nitrite formylation synthesis of methyl formate reaction and carbon monoxide and nitrite The application in the reaction of synthesizing dimethyl oxalate belongs to the technical field of catalysis. Background technique [0002] Dimethyl carbonate (Dimethyl carbonate), referred to as DMC, is a colorless and transparent liquid with a slight fragrance at normal temperature and pressure. Dimethyl carbonate is an environmentally friendly organic chemical raw material that meets the requirements of mo...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/58B01J27/24B01J35/06B01J35/10B01J37/02B01J37/08B01J37/10C07C67/36C07C68/00C07C69/06C07C69/36C07C69/96
CPCC07C67/36C07C68/00B01J23/44B01J23/58B01J27/24B01J37/0201B01J37/082B01J37/10B01J35/58B01J35/60C07C69/96C07C69/36C07C69/06
Inventor 路勇贾迎帅徐彬萧锦诚王纯正赵国锋
Owner ECO ENVIRONMENTAL ENERGY RES INST
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