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Preparation method of Fe/Mo-Al2O3 catalyst and method of synthesizing leaf alcohol by virtue of piperylene

A technology of mo-al2o3 and piperylene, applied in the direction of physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problems of harsh reaction conditions, complex processes, production High cost and other issues, to achieve the effect of mild process conditions, high purity, and low equipment requirements

Active Publication Date: 2015-06-10
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention mainly solves the problems of complex process, harsh reaction conditions and high production cost in the prior art, and provides a method for synthesizing leaf alcohol with mild reaction conditions, safe and simple process, long catalyst life and low production cost

Method used

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  • Preparation method of Fe/Mo-Al2O3 catalyst and method of synthesizing leaf alcohol by virtue of piperylene

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preparation example Construction

[0031] 1. Preparation method of catalyst for synthesizing leaf alcohol

[0032] (1) First, 40~160 mesh γ-Al 2 O 3 The carrier is calcined at 200~800℃ for 12~48h to remove γ-Al 2 O 3 Physically adsorbed impurities in

[0033] (2) The treated γ-Al 2 O 3 Immerse in a ferric nitrate solution with a mass concentration of 0.1-10% for 12 to 48 hours, filter, wash the filter cake with distilled water for 2 to 50 minutes, and finally place it in a muffle furnace at 300 to 800°C for 3 to 12 hours to obtain a sample of Fe- Al 2 O 3 ;

[0034] (3) The obtained Fe-Al 2 O 3 Immerse in ammonium molybdate solution with a mass concentration of 0.3-10% for 12~48h, filter, wash the filter cake with distilled water for 2~50min, dry at 30~200℃ for 4~48h, and finally put it in a muffle furnace at 300~800℃ Fe / Mo-Al can be obtained by calcination for 2-12h 2 O 3 catalyst.

[0035] 2. Method for synthesizing leaf alcohol with the catalyst of the present invention

[0036] 1. Synthesis of intermediates

[0037]...

Embodiment 1

[0047] 1. The catalyst preparation is carried out in the following order:

[0048] (1) First, 40~60 mesh γ-Al 2 O 3 The carrier is calcined at 200℃ for 12h to remove γ-Al 2 O 3 Physically adsorbed impurities in

[0049] (2) The treated γ-Al 2 O 3 Immerse in 0.1% by mass ferric nitrate solution for 12h, filter, wash the filter cake with distilled water for 2min, and finally put it in a muffle furnace at 300℃ for 3h to obtain the sample Fe-Al 2 O 3 ;

[0050] (3) The obtained Fe-Al 2 O 3 Soaked in 0.3% ammonium molybdate solution for 12h, filtered, washed the filter cake with distilled water for 2min, dried at 30℃ for 4h, and finally placed in a muffle furnace and roasted at 300℃ for 2h to obtain Fe / Mo-Al 2 O 3 catalyst.

[0051] 2. Method of synthesizing leaf alcohol with catalyst

[0052] 1. Synthesis of intermediates

[0053] (1) Combine piperylene and catalyst Fe / Mo-Al 2 O 3 (Fe / Mo-Al 2 O 3 The mass ratio to piperylene is 0.05:1) and the solvent formaldehyde (the mass ratio of piperyle...

Embodiment 2

[0062] 1. The catalyst preparation is carried out in the following order:

[0063] (1) Firstly, 60~10 mesh γ-Al 2 O 3 The carrier is calcined at 500℃ for 36h to remove γ-Al 2 O 3 Physically adsorbed impurities in

[0064] (2) The treated γ-Al 2 O 3 Immerse in a 5% ferric nitrate solution for 36h, filter, wash the filter cake with distilled water for 25min, and finally place it in a muffle furnace at 500℃ for 9h to obtain a sample of Fe-Al 2 O 3 ;

[0065] (3) The obtained Fe-Al 2 O 3 Immerse in a 5% mass concentration of ammonium molybdate solution for 36h, filter, wash the filter cake with distilled water for 25min, dry at 100℃ for 36h, and finally put it in a muffle furnace and roast at 500℃ for 9h to obtain Fe / Mo-Al 2 O 3 catalyst.

[0066] 2. Method of synthesizing leaf alcohol with catalyst

[0067] 1. Synthesis of intermediates

[0068] (1) Combine piperylene and catalyst Fe / Mo-Al 2 O 3 (Fe / Mo-Al 2 O 3 The mass ratio to piperylene is 0.1:1) and the solvent formaldehyde (the mass ra...

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Abstract

The invention relates to a preparation method of a Fe / Mo-Al2O3 catalyst and a method of synthesizing leaf alcohol by virtue of piperylene. The method comprises the following steps: with Fe / Mo as the active component, gamma-Al2O3 as a carrier and formaldehyde or acetaldehyde as a solvent, under the conditions of heating and stirring, catalytically synthesizing 2-methyl-5,6-dihydropyran; and converting 2-methyl-5,6-dihydropyran into the leaf alcohol under the catalysis of alkali metal and amine. According to the method disclosed by the invention, Fe / Mo-Al2O3 is firstly adopted as a catalyst for synthesizing 2-methyl-5,6-dihydropyran through piperylene; according to the process for catalyzed synthesis of 2-methyl-5,6-dihydropyran, conditions are mild, and the equipment requirements are low; Diels-Alder reaction is carried out on piperylene under the action of the catalyst without changing the catalyst; 2-methyl-5,6-dihydropyran, serving as a synthetic intermediate, is subjected to reaction under the catalysis of alkali metal and amine to easily produce leaf alcohol serving as a target product, and purity and yield are high.

Description

Technical field [0001] The invention relates to a method for preparing leaf alcohol, and a method for preparing leaf alcohol using piperylene as a raw material. Especially related to a Fe / Mo-Al 2 O 3 The preparation method of the catalyst and the method for synthesizing leaf alcohol from piperylene. Background technique [0002] Leaf alcohol (chemical name is cis-3-hexen-1-ol) is a very important fragrance, with the natural fragrance of fresh leaves, fresh and natural fragrance, suitable for direct fragrance. Leaf alcohol and its derivatives are one of the world's popular fragrance-type precious spices, and they have also become a symbol of the green revolution in the world's perfume industry. Leaf alcohol and its esters are also indispensable flavoring substances in flavor production. At present, at least 40 kinds of synthetic flavors and flavors contain leaf alcohol. The current world demand is about 200 tons / year. [0003] Leaf alcohol exists in almost all green plants. Howe...

Claims

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Application Information

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IPC IPC(8): B01J23/881C07C33/03C07C29/10C07D309/18
Inventor 肖晓明任海伦肖红张吕鸿李伟宏杨颖
Owner TIANJIN UNIV
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