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Loaded M1-M2-carrier bifunctional catalyst, preparation method and application thereof

A bifunctional catalyst, supported technology, applied in molecular sieve catalysts, amino compound preparation, chemical instruments and methods, etc., can solve problems such as poor universality, and achieve the effect of high catalytic activity and excellent recycling performance.

Inactive Publication Date: 2019-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst has poor applicability to the substrate, and the metal precursor carbonyl compound used is highly toxic

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Weigh 0.1149g of ammonium molybdate tetrahydrate, 0.0195g of citric acid monohydrate, and 25mL of water in a round bottom flask, bathe in water at 60°C for a period of time, then weigh 5g of titanium dioxide and add it to the above solution, and bathe in water at 60°C until The solution was completely evaporated to dryness, dried in an oven at 80°C for 12 hours, ground and placed in a muffle furnace, calcined at 500°C for 3 hours, and the solid was thoroughly ground again. , weigh 0.1294g of ruthenium trichloride trihydrate and dissolve it in 5mL water, add 0.95g of the above solid after 15 minutes in 60°C water bath, continue to 60°C water bath until the solution is completely evaporated, put it in an 80°C oven to dry for 12h, grind it and put it away Put it into a muffle furnace and calcinate at 300°C in air for 2 hours to get 5% Ru-MoO x (1.0) / TiO 2 Catalyst (wherein x=2-3, 1.0 represents with MoO 3 The mass fraction of Mo in the catalyst is 1%), which i...

Embodiment 2

[0033] Example 2: Weigh 0.1149g of ammonium molybdate tetrahydrate, 0.0195g of citric acid monohydrate, and put 25mL of water in a round bottom flask, bathe in water at 60°C for a period of time, add 5g of titanium dioxide to the above solution, and bathe in water at 60°C until The solution was completely evaporated to dryness, dried in an oven at 80°C for 12 hours, ground and put into a muffle furnace, calcined at 500°C for 3 hours, fully ground the solid again, weighed 0.1279g of rhodium trichloride trihydrate and dissolved it in 5mL of water After 15 minutes in 60°C water bath, add 0.95 g of the above solid, continue to 60°C water bath until the solution is completely evaporated to dryness, put it in an 80°C oven for 12 hours, grind it and put it in a muffle furnace, and calcinate it in air at 300°C for 2 hours. 5%Rh-MoO x (1.0) / TiO 2 Catalyst (wherein x=2-3, 1.0 represents with MoO 3 Mo accounted for 1% of the mass fraction of the catalyst) marked as 2# catalyst.

Embodiment 3

[0034]Example 3: Weigh 0.1149g of ammonium molybdate tetrahydrate, 0.0195g of citric acid monohydrate, and 25mL of water in a round-bottomed flask, bathe in water at 60°C for a period of time, add 5g of titanium dioxide to the above solution, and bathe in water at 60°C until The solution was evaporated to dryness completely, and dried in an oven at 80°C for 12 hours. Grind well and put it in a muffle furnace, calcinate at 500°C for 3 hours, grind the solid again, weigh 0.1083g of palladium nitrate hydrate and dissolve it in 5mL of water, add 0.95g of the above solid in a 60°C water bath for 15 minutes, and continue to 60°C Water bath until the solution is completely evaporated, put it in an oven at 80°C for 12 hours, grind it and put it in a muffle furnace, and calcinate it in air at 300°C for 2 hours to get 5% Pd-MoO x (1.0) / TiO 2 Catalyst (wherein x=2-3, 1.0 represents with MoO 3 Mo accounted for 1% of the mass fraction of the catalyst) marked as 3# catalyst.

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PUM

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Abstract

The invention relates to an M1-M2-carrier bifunctional catalyst for selective hydrogenation of amide to prepare an amine compound. Specifically, the component M1 is one or two or more of Ru, Rh, Pd, Ir and Pt, the component M2 is one or two or more of V, Mo, W and Re, and the carrier is mainly a common inorganic oxide or molecular sieve. The content of M1 in the catalyst is 0.1-5wt%, the content of M2 is 0-15wt%, and the inorganic oxide is one or two or more of alumina, magnesium oxide, silica, hydroxyapatite, magnesium-aluminum hydrotalcite, titanium dioxide, cerium oxide and zirconia. The molecular sieve is one or two or more of H-Beta, HZSM-5, NaY and HY. The preparation process includes: impregnating the components M1 and M2 in the carrier at the same time or step by step, and then performing roasting at certain temperature. The catalyst has excellent catalytic performance in the reaction of selective hydrogenation of amide to prepare an amine compound.

Description

technical field [0001] The invention relates to a load type M 1 -M 2 -Supported bifunctional catalyst and its preparation method and application. Background technique [0002] Amine compounds are important fine chemicals, which are widely used in many fields such as dyes, drugs, surfactants, pesticides and organic intermediates. There are many problems in the traditional amide reduction to prepare amine compounds, such as the use of stoichiometric and expensive reducing agents, such as LiAlH 4 , NaBH 4 , silane, etc., and when using the method of catalytic hydrogenation to prepare amine compounds, there are generally disadvantages such as poor selectivity or poor substrate adaptability. Therefore, it is an urgent need to develop a new catalyst that can realize the selective hydrogenation of amides to prepare amines under mild conditions in an environmentally friendly solvent and has a wider range of applicable substrates. [0003] Many patents and literatures have intro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/652B01J23/648B01J23/656B01J29/78C07C209/50C07C211/17C07C211/08C07C211/03C07D295/023C07D295/03C07D295/027
Inventor 王爱琴张帆张磊磊张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI