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Method for supercritically synthesizing leaf alcohol

A supercritical, leaf alcohol technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of high corrosion of equipment, harsh reaction conditions, poor atom economy, etc., and achieve good heat transfer performance. , stable operation, low pollution effect

Active Publication Date: 2010-12-29
SHANDONG NHU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, these methods have one or more of the following disadvantages: long process, low yield, harsh reaction conditions, high corrosion to equipment, and low safety of raw materials
In addition, there is also a shortcoming that the atom economy of these synthetic methods is poor, and a large amount of three wastes will be generated in the synthetic process.

Method used

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  • Method for supercritically synthesizing leaf alcohol
  • Method for supercritically synthesizing leaf alcohol
  • Method for supercritically synthesizing leaf alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-10

[0018] In the supercritical, continuous reaction of n-pentene / formaldehyde in methanol solution under catalyst-free conditions, the yields of different residence times and 3-hexen-1-alcohol relative to formaldehyde are shown in Table 1.

[0019] Table 1 residence time and the relation of the productive rate of 3-hexen-1-alcohol relative formaldehyde

[0020]

[0021] Reaction conditions: n-pentene: formaldehyde = 6 (mol); temperature, 280°C; pressure, 20MPa.

example 11-20

[0023] See Table 2 for the relation between the mol ratio of raw materials and the productive rate of 3-hexen-1-alcohol relative to formaldehyde.

[0024] The relation of the mol ratio of table 2 raw material and the productive rate of 3-hexen-1-alcohol relative formaldehyde

[0025]

[0026] Reaction conditions: temperature, 280°C; pressure, 20MPa; residence time, 30min.

Embodiment 21-30

[0028] Reaction temperature and 3-hexen-1-ol relative formaldehyde productive rate are shown in Table 3.

[0029] The relation of table 3 reaction temperature and the productive rate of 3-hexen-1-alcohol relative formaldehyde

[0030]

[0031] Reaction conditions: n-pentene: formaldehyde = 6 (mol); pressure, 20MPa, residence time, 30min.

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Abstract

The invention discloses a method for supercritically synthesizing leaf alcohol. The conventional methods have one or more of the following defects: long process, low yield, rigorous reaction conditions, high corrosion on equipment and low safety of raw materials. Besides, the conventional methods have a common defect of poor atom economy and a large amount of three wastes generated in the synthesis process. The method for supercritically synthesizing the leaf alcohol comprises the following steps of: uniformly mixing raw materials 1-pentene and formaldehyde in a solvent, adding the mixture into a snake tube reactor, and continuously performing condensation reaction under the supercritical condition; ensuring to enter a flash evaporator through a high pressure valve, cooling low-boiling-point substances flashed out to below 40 DEG C by using a condenser, flowing the low-boiling-point substances into a light component receiver, and flowing the residues into a heavy component receiver; and respectively rectifying and separating the obtained products. The method has the advantages of simple and short process, and only one step reaction; and the continuous synthesis method has the advantages of stable operation, good atom economy and light pollution.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a method for supercritically synthesizing flavor and fragrance leaf alcohol. Background technique [0002] Leaf alcohol (scientific name: cis-3-hexen-1-ol (cis-3-Hexen-1-ol)], the appearance is a colorless oily liquid, with the fragrance of green leaves, slightly soluble in water, soluble in In most organic solvents such as ethanol. The diluted leaf alcohol has the fragrance of fresh grass cut, giving people a feeling of freshness and being in nature. Leaf alcohol and its derivatives are one of the world's most popular fragrance-type precious fragrances. They have been used in at least 40 synthetic fragrances and essences, and have become a symbol of the green revolution in the world's fragrance industry. In view of the important position of leaf alcohol in spices and essences and the huge commercial value brought by it, the research on leaf alcohol has already attracted a...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/38
CPCY02P20/54
Inventor 邱贵生杨芝贾慧明
Owner SHANDONG NHU PHARMA
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