Preparation method of alpha-terpilenol

A technology of terpineol and rectification tower, which is applied in the field of preparation of α-terpineol, can solve the problems of low yield of α-terpineol and inapplicability of solid acid catalyst, and achieve short reaction time and high catalytic efficiency Activity and chemoselectivity, effects of mild conditions

Inactive Publication Date: 2013-04-17
江苏宏邦化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method is to mix the catalyst and raw materials for one-pot reaction, but the reaction of α-pinene to synthesize α-terpineol is a reversible reaction, that is, α-terpineol will lose a molecule of water under acidic conditions to form α- Pinene, one-pot synthesis of α-terpineol yield is not high, and solid acid catalyst is not suitable for tank reactor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Weigh α-pinene (100g), deionized water (100g) and isopropanol (100g) respectively and place in container, heating and boiling produces azeotrope, and azeotrope flows through rectifying tower, condenser Enter the packed tower, the temperature of the packed tower body is 20°C, and react for 20 hours; wherein, the solid acid catalyst of the packed tower is Amberlyst 35 cation exchange resin. Sampling and GC analysis showed that the conversion rate of α-pinene was 92.8%, and the content of α-terpineol was 48.28%.

Embodiment 2

[0018] Embodiment 2: Take alpha-pinene (100g), deionized water (150g) and dioxane (300g) respectively and place in container, heat and boil to produce azeotrope, azeotrope flows through rectification column, condenses The device enters the packed tower, the temperature of the packed tower body is 25°C, and the reaction takes 18 hours; wherein, the solid acid catalyst of the packed tower is NKC-9 cation exchange resin. Sampling and GC analysis showed that the conversion rate of α-pinene was 93.2%, and the content of α-terpineol was 48.52%.

Embodiment 3

[0019] Embodiment 3: Weigh α-pinene (100g), deionized water (200g) and acetone (450g) respectively and place in container, heating and boiling produces azeotrope, and azeotrope flows through rectification tower, condenser and enters filler Tower, packed tower body temperature 30°C, react for 15 hours; wherein, the solid acid catalyst of the packed tower is D72 cation exchange resin. Sampling and GC analysis showed that the conversion rate of α-pinene was 94.8%, and the content of α-terpineol was 48.68%.

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Abstract

The invention discloses a preparation method of alpha-terpilenol, which comprises the steps that firstly, alpha-pinene, water and an organic solvent are placed in a container, and subjected to heating reflux; evaporated vapor enters a rectifying tower; secondly, a gas-phase mixture from the top of the rectifying tower enters a condenser at the top end of the rectifying tower; a condensed liquid enters a packed tower, and hydrated by the catalysis of a solid acid catalyst to form alpha-terpilenol; and finally, a mixed liquid of the packed tower enters the container and is evaporated continuously; the evaporated vapor enters the rectifying tower and separated; alpha-terpilenol is left in the rectifying tower; and a gas phase mixture from the top end of the rectifying tower continuously enters the condenser. The preparation method adopts a rectification-coupling technology, and takes alpha-pinene as a raw material, performs alpha-pinene hydration directly, and produces alpha-terpilenol continuously, the yield of alpha-terpilenol is increased; the selectivity of alpha-terpilenol is improved; the production capacity is improved; the energy consumption and the production cost are lowered; and compared with the traditional technology, the automatization of a production process is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of α-terpineol. Background technique [0002] Terpineol, also known as terpineol, is a spice with a stable lilac aroma. Its aroma has the smell of trees and flowers, which can give people a feeling of being in a secluded forest. It is widely used in spices, essences, cosmetics, and cleaning agents. ﹑Bactericides and foaming agents for flotation minerals. [0003] The synthetic method of terpineol is divided into one-step method and two-step method according to the procedure that reaction is carried out. The one-step method is that α-pinene is hydrated directly under the action of a catalyst to generate terpineol. This method has a short production cycle, but the yield of terpineol is low, there are many by-products, and the purity and aroma are poor; the two-step method is α-pinene Under the action of an acid catalyst, terpene diol hydrate is first obtained, and then terpineol is obtained through catalyti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/14C07C29/00C07C29/80
Inventor 刘兴超吴运福陈文昌王栋周海峰孙伟春徐香桂侯峰黄战鏖陈兆刚
Owner 江苏宏邦化工科技有限公司
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