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Catalyst and preparation method for selective hydrogenation of crotonaldehyde to synthesize crotyl alcohol

A selectivity and catalyst technology, applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of poor stability and easy deactivation of Ir-based catalysts

Inactive Publication Date: 2016-04-20
JINHUA VOCATIONAL TECH COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims at the shortcomings of easy deactivation and poor stability of most existing Ir-based catalysts for preparing crotyl alcohol by selective hydrogenation of gas-phase crotonaldehyde, and provides a modified catalyst with high catalytic efficiency, good reaction selectivity and good reaction stability. Catalyst for selective hydrogenation of crotonaldehyde to crotyl alcohol and preparation method thereof

Method used

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  • Catalyst and preparation method for selective hydrogenation of crotonaldehyde to synthesize crotyl alcohol
  • Catalyst and preparation method for selective hydrogenation of crotonaldehyde to synthesize crotyl alcohol
  • Catalyst and preparation method for selective hydrogenation of crotonaldehyde to synthesize crotyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] ①According to the molar ratio of Fe:Zn:La is 1:0.2:0.2, the total mass percentage of Fe-Zn-La is SiO 2 0.05% of Fe(NO 3 ) 3 9H 2 O and Zn(NO 3 ) 2 ·6H 2 O, La(NO 3 ) 3 ·6H 2 O, add an appropriate amount of water to dissolve and mix well, and the corresponding amount of 2-3mm SiO 2 Add to the mixed solution, shake and soak at room temperature for 10 hours;

[0021] ② Afterwards, evaporate the liquid in an oven at 120°C, and bake it in an air atmosphere at 500°C for 4 hours to obtain Fe-0.2Zn-0.2La / SiO 2 carrier, and then reduced in a hydrogen atmosphere at 500°C for 1 hour.

[0022] ③ SiO according to the mass percentage of Ir 2 3% of the carrier, the molar ratio of Pt:Ir is 0.03, absorb a certain amount of Ir(acac) 3 and Pt(acac) 2 Toluene solution, and mix well, the corresponding amount of Fe-0.2Zn-0.2La / SiO 2 The carrier is added to the mixed solution, stirred evenly, and soaked at room temperature for 3 hours;

[0023] ④ Evaporate the liquid to dryness...

Embodiment 2

[0027] ①According to the molar ratio of Fe:Zn:La is 1:0.5:0.5, the total mass percentage of Fe-Zn-La is SiO 2 0.1% of Fe(NO 3 ) 3 9H 2 O and Zn(NO 3 ) 2 ·6H 2 O, La(NO 3 ) 3 ·6H 2 O, add an appropriate amount of water to dissolve and mix well, and the corresponding amount of 2-3mm SiO 2 Add to the mixed solution, shake and soak at room temperature for 10 hours;

[0028] ② Afterwards, evaporate the liquid in an oven at 120°C, and bake it in an air atmosphere at 500°C for 4 hours to obtain Fe-0.5Zn-0.5La / SiO 2 carrier, and then reduced in a hydrogen atmosphere at 500°C for 1 hour.

[0029] ③ SiO according to the mass percentage of Ir 2 3% of the carrier, the molar ratio of Pt:Ir is 0.03, absorb a certain amount of Ir(acac) 3 and Pt(acac) 2 Toluene solution, and mix well, the corresponding amount of Fe-0.5Zn-0.5La / SiO 2 The carrier is added to the mixed solution, stirred evenly, and soaked at room temperature for 3 hours;

[0030] ④ Evaporate the liquid in a water ba...

Embodiment 3

[0034] ①According to the molar ratio of Fe:Zn:La is 1:0.2:2, the total mass percentage of Fe-Zn-La is SiO 2 0.20% of Fe(NO 3 ) 3 9H 2 O and Zn(NO 3 ) 2 ·6H 2 O, La(NO 3 ) 3 ·6H 2 O, add an appropriate amount of water to dissolve and mix well, and the corresponding amount of 2-3mm SiO 2 Add to the mixed solution, shake and soak at room temperature for 10 hours;

[0035] ② Afterwards, evaporate the liquid in an oven at 120°C, and bake it in an air atmosphere at 500°C for 4 hours to obtain Fe-0.2Zn-2La / SiO 2 carrier, and then reduced in a hydrogen atmosphere at 500°C for 1 hour.

[0036] ③ SiO according to the mass percentage of Ir 2 3% of the carrier, the molar ratio of Pt:Ir is 0.05, absorb a certain amount of Ir(acac) 3 and Pt(acac) 2 Toluene solution, and mix well, the corresponding amount of Fe-0.2Zn-2La / SiO 2 The carrier is added to the mixed solution, stirred evenly, and soaked at room temperature for 3 hours;

[0037] ④ Evaporate the liquid in a water bath ...

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Abstract

The invention relates to a catalyst for synthesizing crotyl alcohol by carrying out selective hydrogenation on crotonaldehyde, and a preparation method of the catalyst. SiO2 with the particle size of 2-3mm is taken as a carrier; a first loading layer is Fe-xZn-yLa, wherein x and y refer to the molar ratios of Zn to Fe and La to Fe respectively, and x=0-5, y=0-5; in the Fe-xZn-yLa / SiO2 carrier, the total mass percent of Fe-Zn-La is 0.05-2.0% of the mass percent of SiO2; Ir-Pt is used as a second loading layer, wherein the mass percent of Ir is 1.0-5.0% of that of SiO2, and the molar ratio of Pt to Ir is 0.03-0.2. The preparation method comprises the steps of firstly, dipping the carrier into a mixed water solution of Fe(NO3)3, Zn(NO3)2 and La(NO3)3; drying by distillation in water bath, calcinating, and reducing to obtain the first loading layer; after that, dipping the first loading layer into a mixed methylbenzene solution of Ir(acac)3 and Pt(acac)2; and drying by distillation in water bath, calcinating, and reducing to obtain 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 the field of chemical catalysts, in particular to a catalyst for selectively hydrogenating crotyl alcohol from crotonaldehyde and a preparation method thereof. Background technique [0002] α, β-unsaturated aldehyde is an important chemical raw material, and the product α, β-unsaturated alcohol obtained by selective hydrogenation of its C=O bond is a raw material and intermediate for spices, medicines, herbicides, coatings, etc. . Crotyl alcohol is a representative compound among α, β-unsaturated alcohols. It is an important intermediate in organic synthesis and is widely used in the manufacture of plastics, plasticizers, herbicides, coatings and pesticides. Therefore, it catalyzes crotonaldehyde The preparation of crotyl alcohol by selective hydrogenation is of great economic value. [0003] The hydrogenation activity of the C=C bond in α,β-unsaturated aldehydes is higher than that of the C=O bond. At the same time, there is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07C33/03C07C29/141
Inventor 洪庆红潘滔陈玲
Owner JINHUA VOCATIONAL TECH COLLEGE
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