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Catalyst for preparing crotyl alcohol from gas-phase crotonaldehyde through selective hydrogenation and preparation method thereof

A crotonaldehyde and selectivity technology, which is applied to the catalyst and preparation field for the selective hydrogenation of gas-phase crotonaldehyde to crotyl alcohol, and can solve the problems of low selectivity and the like

Inactive Publication Date: 2011-11-16
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the disadvantages of low selectivity of most existing Ir-based catalysts for preparing crotyl alcohol by gas-phase hydrogenation, and provides a gas-phase selective hydrogenation of crotonaldehyde with high catalytic efficiency, good reaction selectivity and reaction stability Catalyst for preparing crotyl alcohol and preparation method of the catalyst

Method used

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  • Catalyst for preparing crotyl alcohol from gas-phase crotonaldehyde through selective hydrogenation and preparation method thereof
  • Catalyst for preparing crotyl alcohol from gas-phase crotonaldehyde through selective hydrogenation and preparation method thereof
  • Catalyst for preparing crotyl alcohol from gas-phase crotonaldehyde through selective hydrogenation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] ①Dry TiO in vacuum at 100℃ 2 carrier;

[0022] ② Prepare H at a concentration of 0.007g / ml 2 IrCl 6 solution. Take 0.72ml of H 2 IrCl 6 Add 1gTiO to the solution 2 In the carrier, after stirring evenly, soak at room temperature for 12 hours;

[0023] ③ Then evaporate the liquid to dryness in a water bath at 90°C, and dry at 100°C in a nitrogen atmosphere for 12 hours to obtain a solid powder;

[0024] ④The solid powder in ③ is heated up to 200°C in hydrogen and subjected to reduction treatment for 1 hour, and then the catalyst of the present invention is obtained, wherein the mass percentage of Ir is 0.5%, and Ir is loaded on the carrier TiO 2 superior.

[0025] The test of crotonaldehyde hydrogenation activity is shown in Table 1: under normal pressure, it was inspected in a fixed-bed reactor, the amount of catalyst was 0.2g, the volume ratio of hydrogen / crotonaldehyde was 94:1, the total flow rate was 26ml / min, and the reaction temperature was 60°C .

Embodiment 2

[0027] ①Dry TiO in vacuum at 100℃ 2 carrier;

[0028] ② Prepare H at a concentration of 0.007g / ml 2 IrCl 6 solution. Take 0.72ml of H 2 IrCl 6 Add 1gTiO to the solution 2 In the carrier, after stirring evenly, soak at room temperature for 12 hours;

[0029] ③ Then evaporate the liquid to dryness in a water bath at 90°C, and dry at 100°C in a nitrogen atmosphere for 12 hours to obtain a solid powder;

[0030] ④ heat up the solid powder in ③ to 300° C. for reduction treatment in hydrogen for 1 hour, and then obtain the catalyst of the present invention, wherein the mass percentage of Ir is 0.5%, and Ir is loaded on the carrier TiO 2 superior.

[0031] The test of crotonaldehyde hydrogenation activity is shown in Table 1: under normal pressure, it was inspected in a fixed-bed reactor, the amount of catalyst was 0.2g, the volume ratio of hydrogen / crotonaldehyde was 94:1, the total flow rate was 26ml / min, and the reaction temperature was 80°C .

Embodiment 3

[0033] ①Dry TiO in vacuum at 100℃ 2 carrier;

[0034] ② Prepare H at a concentration of 0.007g / ml 2 IrCl 6 solution. Take 1.44ml of H 2 IrCl 6 Add 1gTiO to the solution 2 In the carrier, after stirring evenly, soak at room temperature for 12 hours;

[0035] ③ Then evaporate the liquid to dryness in a water bath at 90°C, and dry at 100°C in a nitrogen atmosphere for 12 hours to obtain a solid powder;

[0036] ④The solid powder in ③ is heated up to 200°C in hydrogen and subjected to reduction treatment for 1 hour, and then the catalyst of the present invention is obtained, wherein the mass percentage of Ir is 1%, and Ir is loaded on the carrier TiO 2 superior.

[0037] The test of crotonaldehyde hydrogenation activity is shown in Table 1: under normal pressure, it was inspected in a fixed-bed reactor, the amount of catalyst was 0.2g, the volume ratio of hydrogen / crotonaldehyde was 94:1, the total flow rate was 26ml / min, and the reaction temperature was 80°C .

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Abstract

The invention relates to catalyst for preparing crotyl alcohol from gas-phase crotonaldehyde through selective hydrogenation and a preparation method thereof, wherein the carrier of the catalyst is one of TiO2, ZrO2 and ZnO; the active ingredient of the catalyst is a Ir-Ir3+ mixture and the mass percentage content thereof in terms of Ir is 0.5-5%; the Ir-Ir3+ mixture is loaded on the carrier and coexists as metal Ir and IrC13; and the atomic ratio of the Ir element to the Cl element in the catalyst is 1.0-1.5. The preparation method of the catalyst comprises the following steps of: firstly drying the carrier TiO2, ZrO2 or ZnO in vacuum at first, and then adding the carrier to H2IrC16 solution for soaking at the room temperature; next, evaporating the liquid to dryness in a water bath, thereby obtaining powder after drying, and then reducing the obtained powder through reduction using hydrogen, thereby obtaining the catalyst. The catalyst is high in catalytic efficiency, and good in reaction selectivity and reaction stability.

Description

technical field [0001] The invention relates to a chemical catalyst and a preparation method thereof, in particular to a catalyst for selective hydrogenation of gas-phase crotonaldehyde to generate crotyl alcohol and a preparation method thereof. Background technique [0002] The unsaturated alcohols produced by the selective hydrogenation of α, β-unsaturated aldehydes are important raw materials and reaction intermediates in fine chemical production, and are widely used in organic synthesis. Crotyl alcohol is one of the representatives. It is an important organic synthesis intermediate and is widely used in the manufacture of n-butanol, rubber vulcanization accelerators, plastics, plasticizers, herbicides, coatings and pesticides, etc., so crotonaldehyde Selecting hydrogenation to generate crotyl alcohol is of great economic value. [0003] Usually, sodium borohydride, lithium aluminum tetrahydride or aluminum isopropoxide are used to reduce crotonaldehyde to obtain crotyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/135B01J27/138C07C33/03C07C29/141
Inventor 罗孟飞朱琳陈萍谢冠群胡庚申
Owner ZHEJIANG NORMAL UNIVERSITY
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