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Binary amorphous alloy catalyst and preparation method and use thereof

A technology of amorphous alloys and catalysts, applied in the field of binary amorphous alloy catalysts, preparation of catalysts, and amorphous alloy catalysts, can solve problems that have not been reported before, and achieve high conversion rate and selectivity, The effect of excellent catalytic performance

Inactive Publication Date: 2011-09-14
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] After extensive searching of domestic and foreign patent documents and consulting of domestic and foreign publications, there is no report of the same technology

Method used

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  • Binary amorphous alloy catalyst and preparation method and use thereof
  • Binary amorphous alloy catalyst and preparation method and use thereof
  • Binary amorphous alloy catalyst and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) 0.66g InCl 3 4H 2 O was dissolved in 5.0 mL deionized water, and stirred thoroughly to obtain a 0.45 mol / L metal salt solution.

[0023] 2) Add 1.1g KBH at 10°C 4 Dissolve in 10mL deionized water, add dropwise to the above metal salt solution and stir rapidly (800rpm), black particles are gradually formed in the solution, and gas comes out.

[0024] 3) The black particles formed above were washed successively with water and absolute ethanol for 3 to 5 times respectively to obtain an In-B amorphous alloy sample.

[0025] figure 1 For the XRD spectrum of the sample prepared in this example, from the comparison of a and c, it is found that the prepared sample has no crystalline characteristic peaks, and after crystallization at 200 ° C, the characteristic diffraction peaks of metal In appear, slowly stir (500rpm) Some crystallization peaks appeared in the samples prepared under the above conditions; figure 2 For the TEM photo of the sample prepared in this embodim...

Embodiment 2

[0028] Catalyst (represented by In-B-2) prepared in Example 1 is used for the preparation of allyl of p-methyl 1-phenyl-3-butenyl-1-alcohol with respect to methyl benzaldehyde and allyl bromide Alkylation reaction, that is: 1.1mmol In-B catalyst, 0.54g aluminum powder, 2.3mmol p-tolualdehyde, 4.5mmol allyl bromide and 10mL deionized water were added in sequence in a 50mL flask, sealed and heated at a constant temperature. The required reaction temperature is 50° C.; the reaction time is 2.0 h. The separation and analysis of the reaction product are the same as in Example 1. The catalytic performance is shown in Table 1.

Embodiment 3

[0030] The catalyst (represented by In-B-3) prepared in Example 1 is used for the allylation of p-chlorobenzaldehyde and allyl bromide to prepare p-chloro 1-phenyl-3-butenyl-1-alcohol Reaction, that is: add 1.1mmol In-B catalyst, 0.54g aluminum powder, 2.3mmol p-chlorobenzaldehyde, 4.5mmol allyl bromide and 10mL deionized water in a 50mL flask in sequence, heat and keep the temperature at the required reaction The temperature was 50° C.; the reaction time was 2.0 h. The separation and analysis of the reaction products were the same as in Example 1. The catalytic properties are shown in Table 1.

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Abstract

The invention discloses a novel binary indium-boron amorphous alloy catalyst for allylation. The general formula of the catalyst can be represented by InxBy, wherein the sum of x and y is 100, x ranges from 75 to 95 and y ranges from 5 to 25; and the catalyst are spherical particles with a particle size ranging from 5 to 50 nanometers. The preparation method comprises: performing a chemical reduction reaction by regulating the concentration of inorganic salt of indium, keeping temperature between 0 and 20 DEG C and a stirring speed between 600 and 1,000 rpm and adding solution of a hydride ofmetal boron into solution of inorganic salt of indium; and performing centrifugal separation and washing an obtained black solid precipitate in deionized water till the precipitate is neutral. The amorphous alloy provided in the invention can be used as a catalyst for the allylation of compounds such as benzaldehyde and acetophenone in a water phase for preparing enol, has high conversion rate and selectivity in reaction, and has higher catalytic performance than a homogeneous catalyst.

Description

technical field [0001] The invention relates to a binary amorphous alloy catalyst, specifically an amorphous alloy catalyst for allylation reaction, and a preparation method and application of the catalyst, belonging to the technical field of catalysts. Background technique [0002] Allyl alcohol compounds are important basic units of biologically active molecules, such as macrolides, polyethers and antibiotics, all contain allyl alcohol structural units. Organometallic-catalyzed Barbier-type reactions are commonly used to obtain allyl alcohol compounds such as PdCl 2 (PPh 3 ) 2 , but there are problems such as high cost, non-reusable, sensitive to humidity and air, and serious environmental pollution caused by organic solvents. In recent years, for the purpose of sustainable economic and ecological development, organic synthesis in aqueous phase has become one of the research hotspots. The organic reaction in the aqueous phase has: (1) easy and simple to operate, little...

Claims

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Application Information

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IPC IPC(8): B01J23/08C07C33/30C07C29/38
Inventor 李辉董福兴徐烨李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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