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Preparation of isobornyl acetate

A technology of isobornyl acetate and acetic acid, which is applied in the field of preparation of isobornyl acetate, can solve the problems of reduced selectivity, reduced quality, and many harmful impurities, so as to reduce the probability of rearrangement reaction, improve selectivity, highly selective effect

Inactive Publication Date: 2008-12-17
SUZHOU YOUHE SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When these esters are used for esterification with the camphor cycle, molecular rearrangement reactions are prone to occur, thereby reducing the selectivity of the total isobornyl acetate formation, which affects both the quality of camphor and the consumption of raw materials
The refined ester discharged from the bottom of the rectification distillation tower is intermittently and simply vacuum distilled in the finished ester distillation tower. The content of the distilled isobornyl acetate is low, usually only 90-92%, while the remaining light components reach 4-92%. 5%, these light components will further change in the production of camphor, and finally enter the product to cause quality decline
[0008] Visible, the shortcoming of above-mentioned traditional isobornyl acetate manufacturing process is: the selectivity of isobornyl acetate in the esterification reaction is low, and the harmful impurity that generates is many, and target ester selectivity is only 90 ± 2%
The content of isobornyl acetate is low, with more light components, which increases new impurities in camphor, and is difficult to meet the requirements of producing pharmaceutical synthetic camphor

Method used

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  • Preparation of isobornyl acetate
  • Preparation of isobornyl acetate
  • Preparation of isobornyl acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0021] 2250kg of industrial camphene, 1050kg of industrial acetic acid, pumped into the reaction kettle equipped with 10% D001 cationic resin, stirred and reacted for 2 hours, controlled temperature at 22~25°C. According to the chromatographic analysis of the reaction, the content of isobornyl acetate was 74.8%, the content of fennel and 3-camphor was 2.9%, the conversion rate of camphene esterification was 72.4%, and the selectivity of isobornyl acetate was 98.1%.

[0022] The esterification reactants are sent to the refined ester-finished ester series distillation tower for distillation, and the vacuum at the top of the tower is 0.093MPa. The refined ester extracted from the refined ester distillation tower contains 94.8% of isobornyl acetate and 1.3% of terpene light components. The temperature at the bottom of the tower is 130°C, and the isobornyl acetate is extracted from the liquid phase side line in the middle of the finished ester distillation tower. The extraction temp...

Embodiment 2

[0024] 720kg of industrial camphene, 230kg of acetic acid, and 2140kg of camphene solution are pumped into a reaction kettle equipped with 10% D001 cationic resin and stirred for 3.5 hours. The temperature is controlled at 20-25°C with low-temperature water, and the reaction solution is analyzed by chromatography for acetic acid. The isobornyl ester content is 69.5%, the fennel ester is 2.6%, the 3-camphoryl ester is 0.65%, the camphene conversion rate is 68.5%, and the isobornyl acetate selectivity is 97.2%.

[0025] The esterification reactants are sent to the refined ester-finished ester series distillation tower for distillation, the vacuum degree at the top of the tower is 0.093MPa, the temperature of the refined ester extracted from the refined ester distillation tower is 130.2°C, the content of isobornyl acetate is 95.3%, and the light components of terpenes 1.7%, the content of isobornyl acetate extracted from the liquid phase side line in the middle of the finished pro...

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Abstract

The invention discloses a preparation method of isobornyl acetate which is an intermediate needed for producing medical synthetic camphor. The preparation method of the invention takes camphene and acetic acid as raw materials and the isobornyl acetate is prepared under the existence of styrene sulfonic strong acid positive ion resin and according to a certain technological condition. Crude products prepared through the reaction are extracted in a way of liquid phase lateral line by the middle part of a distillation tower of finished ester products after continuous vacuum distillation by a series-wound distillation tower of refined ether and the distillation tower of finished ether products, so as to obtain the isobornyl acetate, namely, the intermediate meeting the requirements for producing the medical synthetic camphor. The preparation method of the invention has the advantages that the continuous distillation of esterified materials can lead the quality of various products within the tower to be stabilized at a quite high level, and the preparation method of the invention has stable operation, low energy consumption, good selectivity of products, little impurity, and high content of the isobornyl acetate.

Description

technical field [0001] The invention relates to a method for producing isobornyl acetate, an intermediate required for the production of medicinal synthetic camphor. High-purity isobornyl acetate is a precondition for synthesizing high-quality medicinal camphor. Background technique [0002] Isobornyl acetate, also known as isobornyl acetate, has a cool and pleasant pine leaf-like aroma, and it can undergo saponification reaction with sodium hydroxide to form isoborneol. [0003] [0004] Isoborneol is converted into camphor by catalytic dehydrogenation, so isobornyl acetate is an important intermediate product for the manufacture of synthetic camphor. [0005] [0006] At present, the production route of isobornyl acetate mainly includes the direct esterification process route of camphene and acetic acid in the presence of a catalyst. Sulfuric acid is usually used as the catalyst, and the reaction temperature is controlled at about 50°C. The initial stage of chemical...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/04
Inventor 刘德生王忠蒋伟民姚健王云桃张亮郑坤生
Owner SUZHOU YOUHE SCI & TECH CO LTD
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