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Multilevel-structure supported nano gold catalyst and preparation method thereof

A catalyst and nano-gold technology, which is applied in the field of multi-level structure nano-material catalysis, can solve the problems that have not been reported in the newspapers.

Active Publication Date: 2013-09-25
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, regarding the anatase TiO with (001) exposed surface 2 There are few reports on nano-gold catalysts as supports, especially the application of this gold catalyst to the catalytic hydrogenation of cinnamaldehyde has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. Preparation of carrier:

[0015] The carrier {001}-xFe-AHSs is obtained using the same preparation method that has been applied for the national invention patent (patent number: 201210208904.4), where x is the metal ion Fe 3+ With Ti 4+ The mole percentage of x is 0.1% to 0.4%.

[0016] Accurately measure 71 ml of isopropanol (IPA) and 0.05 ml of diethylene triamine (DETA) and add them to the beaker, stir gently for 3 minutes until uniformly dispersed, then add 3.35 ml of titanium isopropoxide (TIP) to the above solvent A mixed solution is obtained. Accurately weigh 0.0027 g FeCl 3 ·6H 2 Dissolve O in the mixed solution and disperse it ultrasonically for 3 minutes. Transfer the mixed solution to a 100 ml autogenous pressure reactor, crystallize at 200°C for 24 hours, cool to room temperature after the reaction, then wash the reaction precipitate with absolute ethanol 3 times, and dry at 60°C after washing 12 Hours, a light yellow powder is obtained, and a light yellow p...

Embodiment 2

[0020] 1. Preparation of carrier:

[0021] Accurately measure 71 ml of isopropanol (IPA) and 0.05 ml of diethylene triamine (DETA) and add them to the beaker, stir gently for 3 minutes until uniformly dispersed, then add 3.35 ml of titanium isopropoxide (TIP) to the above solvent A mixed solution is obtained. Accurately weigh 0.0054 g FeCl 3 ·6H 2 Dissolve O in the mixed solution and disperse it ultrasonically for 3 minutes. Transfer the mixed solution to a 100 ml autogenous pressure reactor, crystallize at 200°C for 24 hours, cool to room temperature after the reaction, then wash the reaction precipitate with absolute ethanol 3 times, and dry at 60°C after washing 12 Hours, a light yellow powder is obtained, and a light yellow powder is obtained. Then in a tube furnace in an air atmosphere at a heating rate of 1 ℃ / min to 400 ℃, roasting for 2 hours, the obtained carrier is recorded as {001}-0.2% Fe-AHSs, 0.2% is the metal ion Fe 3+ With Ti 4+ The mole percentage.

[0022] 2. Pr...

Embodiment 3

[0025] 1. Preparation of carrier:

[0026] Accurately measure 71 ml of isopropanol (IPA) and 0.05 ml of diethylene triamine (DETA) and add them to the beaker, stir gently for 3 minutes until uniformly dispersed, then add 3.35 ml of titanium isopropoxide (TIP) to the above solvent A mixed solution is obtained. Accurately weigh 0.0108 g FeCl 3 ·6H 2 Dissolve O in the mixed solution and disperse it ultrasonically for 3 minutes. Transfer the mixed solution to a 100 ml autogenous pressure reactor, crystallize at 200°C for 24 hours, cool to room temperature after the reaction, then wash the reaction precipitate with absolute ethanol 3 times, and dry at 60°C after washing 12 Hours, a light yellow powder is obtained, and a light yellow powder is obtained. Then in a tube furnace in an air atmosphere at a heating rate of 1 ℃ / min to 400 ℃, roasting for 2 hours, the obtained carrier is recorded as {001}-0.4% Fe-AHSs, 0.4% is the metal ion Fe 3+ With Ti 4+ The mole percentage.

[0027] 2. Pr...

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Abstract

The invention discloses a multilevel-structure supported nano gold catalyst and a preparation method thereof, belonging to the technical field of multilevel-structure nano material catalysis. The catalyst consists of the following elements in percentage by mass: 35.5-45.5% of titanium, 55.5-65.5% of oxygen, 0.1-0.4% of iron and 1.0-5.0% of gold. The nano gold catalyst is prepared through a precipitation method by taking iron-doped anatase TiO2 nano-lamella multilevel microspheres with a high (001) crystal face exposure rate as a carrier, wherein strong metal-carrier interaction exists between nano gold and the carrier, and the catalyst is suitable for alpha, beta-unsaturated aldehyde / ketone liquid phase selective hydrogenation reaction. When the reaction temperature is 120 DEG C and the pressure is 1.0MPa, H2 is used as a reducing agent for reacting for 2 hours, the conversion rate of a catalytic cinnamic aldehyde hydrogenation reaction is 75-80%, and the selectivity of cinnamic alcohol is 60-70%.

Description

Technical field [0001] The invention belongs to the technical field of multi-level structure nano material catalysis, and in particular provides a multi-level structure supported nano-gold catalyst and a preparation method thereof. The iron-doped anatase titanium dioxide nano-sheets with high (001) crystal face exposure rate Multi-level structure supported nano-gold catalyst with multi-level microspheres as carrier. Background technique [0002] The selective hydrogenation of α, β-unsaturated aldehydes / ketones is a key step in the production and synthesis of fine chemicals. The hydrogenated products of unsaturated alcohols are important raw materials for the production of pharmaceutical intermediates and spices. However, the methods commonly used in the industry currently have disadvantages such as harsh reaction conditions, large amount of reducing agent, difficult separation of products, and serious problems with the discharge of three wastes. The method of heterogeneous catal...

Claims

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Application Information

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IPC IPC(8): B01J23/745C07C33/32C07C29/141
Inventor 张慧刘婷钟丽
Owner BEIJING UNIV OF CHEM TECH
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