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Method for preparing methyl-2-buten-1-ol from 3-methylcrotonaldehyde by selective hydrogenation

A technology of prenyl aldehyde and prenol, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problem of high reaction temperature and pressure, high price and low space velocity of prenol And other problems, to achieve the effect of good activity stability, long operation time, and reduce production cost

Inactive Publication Date: 2019-02-22
杭州更蓝生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the invention is to provide a method for preparing prenol by prenyl aldehyde selective hydrogenation, that is, use a loaded Al-Zn / CeO The method for preparing prenol by prenyl aldehyde selective hydrogenation solves the problem of Problems such as high reaction temperature and pressure and low space velocity of isopentenol caused by expensive supported palladium or platinum catalyst

Method used

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  • Method for preparing methyl-2-buten-1-ol from 3-methylcrotonaldehyde by selective hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Mix and stir a certain amount of aluminum nitrate, zinc tetrachloride and deionized water evenly to obtain an impregnation solution containing Al-Zn; add a certain amount of α-CeO2 carrier to the above impregnation solution, let it stand for aging at room temperature for 24 hours, and then pass through Drying at 80°C for 4h, calcining at 700°C for 4h, to obtain Catalyst I;

[0028] The catalyst precursor is reduced, the reduction temperature is 400°C, the reduction time is 10h, the hydrogen content in the hydrogen-containing atmosphere is 15% by volume, and the volume space velocity of the hydrogen-containing atmosphere is 2000h -1 , to obtain catalyst I. By adjusting the amount of active component and carrier, the composition of catalyst I is: Al content 11.5% by weight, Zn content 9.3% by weight, α-CeO2 content 79.2% by weight.

Embodiment 2

[0030] Mix and stir a certain amount of aluminum nitrate, zinc tetrachloride and deionized water evenly to obtain an impregnating solution containing Al-Zn; add a certain amount of gamma-CeO2 carrier to the above impregnating solution, let it stand for aging at room temperature for 24 hours, and then pass through Drying at 80°C for 4h, and calcining at 700°C for 4h to prepare the catalyst precursor;

[0031] The catalyst precursor is reduced, the reduction temperature is 400°C, the reduction time is 10h, the hydrogen content in the hydrogen-containing atmosphere is 15% by volume, and the volume space velocity of the hydrogen-containing atmosphere is 2000h -1 , to obtain Catalyst II. By adjusting the amount of active components and supports, the composition of the catalyst II is: the content of Al is 13.2% by weight, the content of Zn is 8.8% by weight, and the content of γ-CeO2 is 78% by weight.

Embodiment 3

[0033] Mix and stir a certain amount of aluminum nitrate, zinc tetrachloride and deionized water evenly to obtain an impregnating solution containing Al-Zn; add a certain amount of gamma-CeO2 carrier to the above impregnating solution, let it stand for aging at room temperature for 24 hours, and then pass through Drying at 80°C for 4h, and calcining at 700°C for 4h to prepare the catalyst precursor;

[0034] The catalyst precursor is reduced, the reduction temperature is 400°C, the reduction time is 10h, the hydrogen content in the hydrogen-containing atmosphere is 15% by volume, and the volume space velocity of the hydrogen-containing atmosphere is 2000h -1 , to obtain catalyst III. By adjusting the amount of active components and supports, the composition of the catalyst III is as follows: the content of Al is 8.6% by weight, the content of Zn is 12.1% by weight, and the content of γ-CeO2 is 79.3% by weight.

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Abstract

The invention discloses a method for preparing methyl-2-buten-1-ol from 3-methylcrotonaldehyde by selective hydrogenation. The method comprises steps as follows: 3-methylcrotonaldehyde and hydrogen are mixed under the conditions of temperature being 50-80 DEG C, pressure being 0.1-3.0 MPa, mass space velocity being 5-8 h<-1> and a ratio of feeding substance amount of hydrogen to 3-methylcrotonaldehyde being 1:1-20:1, a mixture is contacted with a supported Al-Zn / CeO2 catalyst for a hydrogenation reaction, and methyl-2-buten-1-ol is obtained. The catalyst is cheaper and has high selective activity, methyl-2-buten-1-ol can be prepared under the conditions of low temperature, low pressure and high space velocity, and production cost of methyl-2-buten-1-ol is reduced.

Description

technical field [0001] The invention relates to the field of organic chemical industry, in particular to a method for preparing prenol by selective hydrogenation of prenyl aldehyde. Background technique [0002] Isopentenol (3-methyl-2-butenol), is an important medicine, fragrance and pesticide intermediate, which can be used in the production of citral, isophytol, DV methyl chrysanthemum, vitamin E, vitamin A. Carotenoid intermediates, etc., can also be used in other organic synthesis. [0003] The synthetic method of isopentenol mainly contains following several kinds at present: [0004] 1. Isobutene method: Patent US4028424 describes the preparation of prenol by Prince reaction with isobutene and formaldehyde as raw materials, but the selectivity of this reaction is poor, the selectivity of prenol is about 5%, and 80 ~90% 3-methyl-3-butenol; [0005] Patent WO2008037693 describes that 3-methyl-3-butenol is prepared by condensation reaction using isobutene and formalde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/141C07C33/025B01J23/10
CPCB01J23/10C07C29/141C07C33/025Y02P20/584
Inventor 董秋月杨彩花
Owner 杭州更蓝生物科技有限公司
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