Method for preparing isoamyl aldehyde from 3-methyl-3-butenyl-1 alcohol

A technology of butenyl and isovaleraldehyde, which is applied in the field of photocatalytic reaction for preparing isovaleraldehyde, can solve the problems of difficult control of oxygen supply, high catalyst preparation and cost, short service life, etc., and achieves high conversion rate of effective products, Conducive to the implementation of industrialization, the method is scientific and reasonable

Inactive Publication Date: 2015-09-23
吉林众鑫化工集团有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese Patent Publication (Announcement) No. CN1566056A discloses the name as: the preparation method of isovaleraldehyde, the adopted isoamyl alcohol raw material is technical grade, and its source is few, and isoamyl alcohol majority has 2,3 position isomers to exist, Low purity of technical grade isoamyl alcohol
There is an existing method for preparing isovaleraldehyde using Ag / KZSM-5 molecular sieve as a catalyst, but the preparation and cost of the catalyst are high, the service life is short, the production energy consumption is high, and the oxygen supply in the reaction is difficult to control. big security risk

Method used

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  • Method for preparing isoamyl aldehyde from 3-methyl-3-butenyl-1 alcohol
  • Method for preparing isoamyl aldehyde from 3-methyl-3-butenyl-1 alcohol
  • Method for preparing isoamyl aldehyde from 3-methyl-3-butenyl-1 alcohol

Examples

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Effect test

Embodiment 1

[0012] Example 1: 196g of 3-methyl-3-butenyl-1-alcohol and 4.0g of catalyst were mixed and stirred evenly and added to a 500ml reactor, and placed at a temperature of 140 ℃ The reactor in the oil bath pot, feed nitrogen into the material under normal pressure, replace the air in the reactor to make it anaerobic, and then heat it to the required reaction temperature, 110°C-130°C, in the ultraviolet The reaction starts under light irradiation, and as the reaction progresses, part of the product isovaleraldehyde evaporates through the cooling device on the reactor, and is continuously separated to obtain part of the crude product of isovaleraldehyde; the total reaction time is 3-4h, and the reaction raw materials are all converted The desired products isovaleraldehyde and 3-methyl-2-butenyl-1-ol with a small amount of isopentyl alcohol by-product. After the reaction is finished, the reaction product is rectified by a rectification tower to obtain high-purity isovaleraldehyde and ...

Embodiment 2

[0018] Example 2, 1.572 kg of 3-methyl-3-butenyl-1-ol and 28 g of catalyst were mixed and stirred evenly and added to a 2L reactor, and an ultraviolet lamp was added to a hollow position inside the reactor to pass through the ultraviolet lamp at 254nm Light irradiation, place the reactor in an oil bath at a temperature of 140°C, pass nitrogen into the material under normal pressure, replace the air in the reactor to make it in an anaerobic state, and then heat it to the required reaction temperature of 110°C -130°C, the reaction starts under the irradiation of ultraviolet light. As the reaction progresses, part of the product isovaleraldehyde evaporates through the cooling device on the reactor, and is continuously separated to obtain part of the crude product of isovaleraldehyde; the total reaction time is 3- 4h, the reaction raw materials were all converted to generate the desired product isovaleraldehyde and 3-methyl-2-butenyl-1-ol and a small amount of impurity by-products....

Embodiment 3

[0022] Example 3, 6.895kg of 3-methyl-3-butenyl-1-ol and 105g of catalyst were mixed and stirred evenly and added to a 10L reactor, and an ultraviolet light was added to a hollow position inside the reactor to pass through the ultraviolet light at 254nm Irradiate, place the reactor in the oil bath at a temperature of 140°C, pass nitrogen into the material under normal pressure, replace the air in the reactor to make it in an anaerobic state, and then heat it to the required reaction temperature of 110°C- 130°C, the reaction starts under the irradiation of ultraviolet light. As the reaction progresses, part of the product isovaleraldehyde evaporates through the cooling device on the reactor, and is continuously separated to obtain part of the crude product of isovaleraldehyde; the total reaction time is 3-4h , the reaction raw materials are all converted to generate the desired product isovaleraldehyde and 3-methyl-2-butenyl-1-alcohol and a small amount of impurity by-products. ...

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Abstract

The invention discloses a method for preparing isoamyl aldehyde from 3-methyl-3-butenyl-1 alcohol. The method is characterized by comprising the following steps: putting raw materials comprising 98-98.5 percent (in percentage by mass) of 3-methyl-3-butenyl-1 alcohol and 1.5-2 percent of an organic metal compound catalyst into a reactor; putting the reactor into an oil bath pan of 140 DEG C under normal pressure to carry out heating reaction at a temperature of 110-130 DEG C; under a N2 atmosphere anoxic condition, continuously separating part of isoamyl aldehyde generated in a photo-catalytic reaction process by distilling, promoting reaction for generating isoamyl aldehyde to further positively carry out, wherein the total reaction time is 3-4 hours; finally, obtaining high-purity isoamyl aldehyde, 3-methyl-3-butenyl-1 alcohol and a little isoamyl alcohol by carrying out separation, rectification and purification on all crude product. The method is scientific and reasonable, low in reaction temperature and pressure, high in effective product conversion rate, energy-saving and low in production cost.

Description

technical field [0001] The invention relates to a method for preparing isovaleraldehyde with 3-methyl-3-butenyl-1 alcohol, in particular to a method for preparing isovaleraldehyde by photocatalytic reaction under normal pressure organometallic compound catalyst conditions. Background technique [0002] The chemical name of isovaleraldehyde is 3-methylbutyraldehyde. Its main application is rubber accelerator, organic synthesis and artificial fragrance. Isovaleraldehyde is a raw material for producing isovaleric acid, an intermediate for synthesizing fragrances, and a raw material in the food industry and pharmaceutical industry. Especially as a synthetic raw material for vitamin E, it is used in a huge amount. Isovaleraldehyde occurs naturally in essential oils such as citrus and lemon. It has an apple-like aroma when highly diluted, and a peach-like aroma when the concentration is lower than 10ppm. my country's GB2760-86 stipulates that it is an edible spice that is allow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/02C07C45/51C07C33/03C07C29/56
CPCC07C45/512C07C29/56
Inventor 孙东日汪颖陈迪伟李薇邹灵俊
Owner 吉林众鑫化工集团有限公司
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