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Method for producing high-purity isoborneol

An isoborneol and high-purity technology, applied in the field of producing high-purity isoborneol, can solve the problems of large amount of camphene, high cost, large centrifugal workload, etc., and achieves less amount of camphene, low cost, and reduced labor intensity. Effect

Inactive Publication Date: 2012-02-08
FUJIAN GREEN PINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The purity of the isoborneol produced by this method is about 80-90%, the product is slightly yellowish, and the amount of camphene needed for production is large, the cost is high, and the centrifugal workload is large

Method used

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  • Method for producing high-purity isoborneol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Saponification reaction: The isobornyl acetate with a content of ≥97% produced by the esterification of camphene and acetic acid is pumped to the saponification reactor E-101, and a 30% sodium hydroxide solution is added to ≥98% xylene, feed isobornyl acetate: sodium hydroxide solution: xylene = 4:3:1, heat up to 150°C, and control the pressure at 0.30MPa. After reacting for 8 hours, take a sample for analysis. The reaction can be stopped if the bornyl ester content is ≤0.5%, and the cooling water is passed into the jacket of the saponification reaction kettle to cool down the temperature of the feed liquid.

[0023] (2) Water washing: add 10% sodium acetate solution into saponification reactor E-101, stir for 5 minutes, let it stand for 5 minutes, then enter 80% sodium acetate solution into water washing tank E-102, and wash until pH=7.

[0024] (3) Dehydration: Stir the feed liquid in the saponification reactor E-101 and raise the temperature to 120°C. Water and x...

Embodiment 2

[0028] (1) Saponification reaction: Isobornyl acetate with a content ≥ 97% generated by the esterification reaction of camphene and acetic acid is pumped to the saponification reactor E-101, and sodium hydroxide solution with a mass fraction of 46% is added. ≥98% xylene, according to isobornyl acetate: sodium hydroxide solution: xylene = 4.2:3.5:1 feed, temperature rises to 155°C, pressure is controlled at 0.35MPa, after 10 hours of reaction, sampling analysis, acetic acid iso The reaction can be stopped if the bornyl ester content is ≤0.5%, and the cooling water is passed into the jacket of the saponification reaction kettle to cool down the temperature of the feed liquid.

[0029] (2) Washing: Add 15% sodium acetate solution into saponification reactor E-101, stir for 5 minutes, let it stand for 10 minutes, then enter 85% sodium acetate solution into water washing tank E-102, and wash until pH=7-8.

[0030] (3) Dehydration: Stir the feed liquid in the saponification reactor ...

Embodiment 3

[0034] (1) Saponification reaction: Isobornyl acetate with a content of ≥97% produced by the esterification of camphene and acetic acid is pumped to the saponification reactor E-101, and sodium hydroxide solution with a mass fraction of 38% is added. ≥98% xylene, according to isobornyl acetate: sodium hydroxide solution: xylene = 4.1:3.2:1 feed, temperature rises to 152°C, pressure is controlled at 0.32MPa, after 9 hours of reaction, sampling analysis, acetic acid iso The reaction can be stopped if the bornyl ester content is ≤0.5%, and the cooling water is passed into the jacket of the saponification reaction kettle to cool down the temperature of the feed liquid.

[0035] (2) Washing: add 12% sodium acetate solution into the saponification reactor E-101, stir for 5 minutes, let it stand for 8 minutes, enter the 83% sodium acetate solution into the washing tank E-102, and wash until pH=7-8.

[0036] (3) Dehydration: Stir the feed liquid in the saponification reactor E-101 and...

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Abstract

The invention discloses a method for producing high-purity isoborneol, which comprises the following steps: carrying out saponification reaction on isoborneol acetate and a sodium hydroxide solution to generate an isoborneol solution; and vaporizing the isoborneol solution, purifying by fractionation, and subliming to obtain the white crystal or powder isoborneol. The purity of the isoborneol produced by the method disclosed by the invention is higher than 95%, and the isoborneol is brilliant white in color. The invention has the advantages of low cost, simple technique, no need of centrifugation, energy saving and environmental protection.

Description

technical field [0001] The invention belongs to the field of compound synthesis, in particular to a method for producing high-purity isoborneol. Background technique [0002] Isoborneol is a forestry chemical product. Isoborneol is also called isoborneol, and its properties are similar to camphor. The isoborneol produced by the method has a good white appearance. Uses: It is used as a spice in daily chemical products, and also as a preservative. The appearance and properties of white isoborneol are similar to camphor, and the cost is relatively low. The application prospect is very broad. [0003] The current production process of isoborneol adopts the hydration method, that is, under the catalysis of resin, camphene, isopropanol and dilute acid are hydrated in proportion to obtain crude isoborneol, and then centrifuged to obtain pure isoborneol. The purity of the isoborneol produced by this method is about 80-90%, the product is slightly yellowish, and the amount of camph...

Claims

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Application Information

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IPC IPC(8): C07C35/30C07C27/02C07C29/76C07C29/80
Inventor 陈尚和危景波邓新贵王志林
Owner FUJIAN GREEN PINE
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