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Method for preparing isoborneol through continuous saponification of isobornyl acetate

A technology of isoborneol acetate and isoborneol, applied in the chemical field, can solve the problems of high energy consumption, complicated saponification process, long reaction time, etc., to reduce the discharge of waste liquid, shorten the reaction time, and be conducive to sustainable production effect

Active Publication Date: 2015-04-01
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, indirect method is mostly used in industrial synthesis to synthesize isoborneol, but its saponification reaction is intermittent operation, which has the disadvantages of complex saponification process, long reaction time, high energy consumption and low yield.

Method used

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  • Method for preparing isoborneol through continuous saponification of isobornyl acetate

Examples

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Embodiment 1

[0035] A method for preparing isoborneol by continuous saponification of isoborneol acetate, specifically comprising the following steps:

[0036] 1) Pump the sodium hydroxide aqueous solution (1) with a mass fraction of 46% and the polar solvent acetone (2) into the polar solution storage tank V-101, mix and stir evenly, and prepare a polar solution; the hydroxide The molar ratio of sodium aqueous solution to acetone is 1:3;

[0037] 2) According to the molar ratio of isobornyl acetate and sodium hydroxide as 1:1.2, pump the polar solution of isobornyl acetate (3) and step 1) into such as figure 1 In the oscillatory flow reactor R-101, the circulating water temperature is stabilized to 80°C, and the oscillatory pump P-101 is turned on at the same time, the oscillation frequency is adjusted to 4Hz, the oscillation amplitude is 0.03m, and the saponification reaction is 30 minutes; the purity of the isobornyl acetate 97.8%;

[0038] 3) When the height of the raw material liqu...

Embodiment 2

[0044] A method for preparing isoborneol by continuous saponification of isoborneol acetate, specifically comprising the following steps:

[0045] 1) Pump sodium hydroxide aqueous solution (1) with a mass fraction of 40% and polar solvent methanol (2) into the polar solution storage tank V-101, mix and stir evenly, and prepare a polar solution; the hydroxide The molar ratio of sodium aqueous solution to methanol is 1:1.4;

[0046] 2) According to the molar ratio of isobornyl acetate and sodium hydroxide as 1:1.15, pump the polar solution of isobornyl acetate (3) and step 1) into such as figure 1 The oscillating flow reactor R-101 stabilizes the temperature of the circulating water to 70 ° C, and at the same time starts the oscillating pump P-101, adjusts the oscillation frequency to 3 Hz, the oscillation amplitude to 0.05 m, and saponifies for 25 min; the purity of the isobornyl acetate 97.3%;

[0047] 3) When the height of the raw material liquid in the reactor reaches the...

Embodiment 3

[0053] A method for preparing isoborneol by continuous saponification of isoborneol acetate, specifically comprising the following steps:

[0054] 1) Pump sodium hydroxide aqueous solution (1) with a mass fraction of 30% and polar solvent isopropanol (2) into the polar solution storage tank V-101, mix and stir evenly, and prepare a polar solution; The molar ratio of sodium hydroxide aqueous solution to isopropanol is 1:6;

[0055] 2) According to the molar ratio of isobornyl acetate and sodium hydroxide as 1:1.1, pump the polar solution of isobornyl acetate (3) and step 1) into such figure 2 Static mixer R-101, the circulating water temperature is stabilized to 60 ° C, saponification reaction 10 min; the purity of the isobornyl acetate is 97.1%;

[0056] 3) When the height of the raw material liquid in the reactor reaches the height of the non-polar solvent inlet, according to the molar ratio of isobornyl acetate, non-polar solvent and water as 1:2:6, the non-polar solvent d...

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Abstract

The invention discloses a method for preparing isoborneol through continuous saponification of isobornyl acetate. Sodiumhydroxide and the isobornyl acetate are used as raw materials, and white isoborneol crystals are prepared through steps of saponification, rectification, layering, water washing, crystallization and the like. Continuous operation of a saponification reaction can be realized in an oscillatory flow reactor, a static mixer or an ultrasonic mixer; a polar solvent is added during reaction, so that the saponification reaction is conducted at a homogeneous phase, the reaction time can be shortened, the reaction temperature can be reduced, the conversion rate of the isobornyl acetate exceeds 99%, and the product yield exceeds 95%; the method is low in energy consumption for production and high in product yield.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing isoborneol by continuous saponification of isoborneol acetate. Background technique [0002] Isoborneol, also known as isoborneol, is a forest chemical product and an epimer of borneol, with molecular formula C 10 h 18 O. Isoborneol has a special smell and can be used in the fields of spices and medicine, and is an intermediate in the synthesis of camphor. [0003] At present, the synthesis methods of isoborneol in industry mainly include indirect method and direct method. The direct method is to directly hydrate amphene to generate isoborneol under the action of an acidic catalyst, which has the advantages of simplifying the steps and saving raw materials, but the conversion rate and selectivity are relatively low. The indirect method is to generate isoborneol acetate by esterifying camphene with acetic acid, and then saponify isoborneol ac...

Claims

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Application Information

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IPC IPC(8): C07C35/30C07C27/02C07C29/80
CPCC07C29/095C07C29/12C07C29/76C07C29/78C07C29/80C07C29/86C07C2602/42C07C35/30
Inventor 郑辉东胡以超严佐毅王碧玉
Owner FUZHOU UNIV
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