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Improved process for preparing isobornyl acetate

A technology of isoborneol acetate and acetic acid is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effect of reducing preparation cost and improving yield

Inactive Publication Date: 2011-05-11
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

"Forest Products Chemistry and Industry" Vol.9No.1p19-26, has reported the method for preparing isobornyl acetate from camphene with cationic resin fixed bed catalysis, which makes the original batch operation continuous, but its single pass yield (reaction optional) there is still room for improvement

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  • Improved process for preparing isobornyl acetate
  • Improved process for preparing isobornyl acetate
  • Improved process for preparing isobornyl acetate

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Embodiment 1

[0016] A shell-and-tube fixed-bed reactor is used, and the size of the reaction tube is 44×2×3000 mm, 22 pieces, catalyst volume: 78 liters. Raw material flow rate: 1.0-2.4 liters / min. Raw material processing capacity: 1440-3401 liters / day, about 1576-3723kg (weight ratio of camphene and acetic acid is 1:1.5) / day.

[0017] At a reaction temperature of 40°C, the preferred space velocity is 0.02min -1 . The product analysis values ​​are shown in Table 2 below (measuring instrument: gas chromatograph (GC900C), chromatographic column specification: PEG-20M chromatographic column, column oven temperature: 140°C, gasification chamber temperature: 250°C, detector temperature: 250°C, Hydrogen: 0.12Mpa, Nitrogen: 0.26Mpa, Air: 0.07Mpa).

[0018] Table 2

[0019]

[0020] Under above-mentioned same condition, be that 50-55% acidic cation exchange resin is catalyzer with water content, the analytical value of gained product is shown in Table 3:

[0021] table 3

[0022]

[...

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Abstract

The invention relates to a method for preparing isobornyl acetate by the reaction of camphene and acetic acid. The method comprises the following main steps: the camphene reacts with the acetic acid in the presence of acidic cation exchange resin to obtain the target product. The method is characterized in that based on the total weight of the acidic cation exchange resin, the moisture content ofthe acidic cation exchange resin is less than or equal to 10wt%. In the method, the yield of the isobornyl acetate (the yield of the isobornyl acetate is more than 80%) is improved and the preparation cost of the isobornyl acetate is lowered by controlling the moisture content of the reaction system, especially strictly controlling the moisture content of the catalyst, thus laying a foundation for the large-scale commercial preparation of the isobornyl acetate.

Description

technical field [0001] The present invention relates to a kind of preparation method of isobornyl acetate, specifically, relate to a kind of method of preparing isobornyl acetate by camphene and acetic acid reaction. Background technique [0002] Camphor is a terpenoid compound belonging to a bicyclic monoterpene. The synthesis of camphor has important significance in organic synthesis. Due to the increasing scarcity of natural camphor resources, synthetic camphor has been paid more and more attention. [0003] Isobornyl acetate is an important intermediate for the preparation of camphor. "Forest Products Chemistry and Industry" Vol.9No.1p19-26, has reported the method for preparing isobornyl acetate from camphene with cationic resin fixed bed catalysis, which makes the original batch operation continuous, but its single pass yield (reaction selectivity) there is still room for improvement. Contents of the invention [0004] The object of the present invention is to pr...

Claims

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Application Information

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IPC IPC(8): C07C69/03C07C69/12C07C67/04
Inventor 刘殿华房鼎业蒋晓庄黄鑫陈瑾
Owner EAST CHINA UNIV OF SCI & TECH