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Production method of dihydromyrcenol

A technology for dihydromyrcenol and dihydromyrcene, which is applied in the field of producing dihydromyrcenol, can solve the problems of poor selectivity, high energy consumption, low conversion rate and the like, achieves inhibition of isomerization and saves total energy consumption , the effect of reaction conversion and selectivity improvement

Active Publication Date: 2013-03-13
NANJING ENETEKS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the process has problems such as low conversion rate (about 1.5-3% per hour, calculated as DHM), poor selectivity (up to 90%) and high energy consumption, so new processes must be developed to overcome the above shortcomings

Method used

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  • Production method of dihydromyrcenol

Examples

Experimental program
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Effect test

Embodiment 1

[0035]In the catalyst fixed bed layer 4 of the IRRFB reactor 3, the catalyst strong acid ion exchange resin Amberlyst15 (provided by Rohm and Haas company in the United States) is filled, and dihydromyrcene, water and chloroform are respectively input through the DHM feed pipe 1 and water and solvent The tube 2 enters the forced circulation radiant flow fixed bed (IRRFB for short) reactor 3, the mass ratio of DHM, water and chloroform solvent is 1:1:1, and it is preheated by the preheater to reach the reaction temperature of 60°C respectively. The pressure is 0.2MPa, and the catalyst loading in the catalyst fixed bed 4 is 25% of the reactor volume. The distance between the outer wall surface of the catalyst fixed bed 4 and the inner wall surface of the reactor is 60mm. The central pipe 5 has the same diameter as the second pipe 8 . The catalyst thickness of the catalyst fixed bed 4 (approximately equal to the distance between the inner wall and the outer wall) is 100 mm. The...

Embodiment 2

[0040] In the catalyst fixed bed layer 4 of the IRRFB reactor 3, the catalyst strong acid ion exchange resin Amberlyst36 (provided by Rohm and Haas, USA) is filled, and dihydromyrcene, water and chloroform are input through the DHM feed pipe 1 and water and solvent respectively Tube 2 enters the forced circulation radiant flow fixed bed (hereinafter referred to as IRRFB) reactor 3, the mass ratio of DHM, water and chloroform solvent is 1:0.5:1, and it is preheated by the preheater to reach the reaction temperature of 58°C respectively. The pressure is 0.18MPa, and the catalyst loading in the catalyst fixed bed 4 is 25% of the reactor volume. The distance between the outer wall surface of the catalyst fixed bed 4 and the inner wall surface of the reactor is 60mm. The central pipe 5 has the same diameter as the second pipe 8 . The catalyst thickness of the catalyst fixed bed 4 (approximately equal to the distance between the inner wall and the outer wall) is 100mm. The overall...

Embodiment 3

[0044] In the catalyst fixed bed 4 of the IRRFB reactor 3, the catalyst strong acid ion exchange resin Amberlyst15 is packed, and dihydromyrcene, water and methyl ethyl ketone enter into the forced In the circulating radiant flow fixed bed (IRRFB for short) reactor 3, the mass ratio of DHM, water and methyl ethyl ketone solvent is 1:0.5:1, and they are preheated by the preheater respectively to reach the reaction temperature of 73°C. The pressure is 0.25MPa, and the catalyst loading in the catalyst fixed bed 4 is 25% of the reactor volume. The distance between the outer wall surface of the catalyst fixed bed 4 and the inner wall surface of the reactor is 60mm. The central pipe 5 has the same diameter as the second pipe 8 . The catalyst thickness of the catalyst fixed bed 4 (approximately equal to the distance between the inner wall and the outer wall) is 100mm. The overall height of the reactor 3 is typically 1600 mm. The flow rate of the circulation pump is V= 50V 0 .

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Abstract

The invention provides a production method of a dihydromyrcenol. The technological processes are shown as the figure and carried out through the following step of: introducing dihydromyrcenol (hereafter referred to as DHM), water and a low-viscosity organic solvent X via a DHM feed pipe 1 and a water and solvent input pipe2 into a forced circulation radiation flow fixed bed (hereafter referred to as IRRFB) reactor 3. The pressure in the reactor is 0.12-0.28MPa; the IRRFB reactor 3 is provided with a barrel-shaped housing; a centre pipe 5 with two sealed ends and apertures covered on a side wall is arranged in the housing; and a catalyst fixed bed layer 4 made of metal nets and filled with catalysts is arranged outside the centre pipe 5. A reaction solution is pumped into the centre pipe 5, is introduced into the catalyst fixed bed layer 4 at a high speed in a radiation manner via the apertures on the side wall, penetrates through the catalyst fixed bed layer 4 to enter the housing of the reactor 3 and carries out a next round of circulation via a first pipeline 6 at the bottom. Firstly, oil and water are separated in a reacted liquid and a product is rectified twice, so that a product with a purity of 99.61% is obtained; and the once conversion rate is 10.6%, and the selectivity is 98.1%.

Description

field of invention [0001] The present invention relates to a new method for producing dihydromyrcenol. Background technique [0002] Dihydromyrcenol (2,6-dimethyl-7-octen-2-ol, hereinafter referred to as DHMOH) is an important fragrance with strong fruity, floral, green, woody and white lemon Fragrance, fragrance has good stability in soap and detergent. Due to its unique aroma quality, it is widely used in flavor formulations and has a very broad market prospect. At present, DHMOH products are mainly obtained by hydrating dihydromyrcene (hereinafter referred to as DHM) in a traditional fixed-bed reactor. This process mostly uses isopropanol, dioxane, butanol, ethylene glycol monobutyl ether, etc. as DHM hydration solvent. However, the process has problems such as low conversion rate (about 1.5-3% per hour, calculated as DHM), poor selectivity (up to 90%) and high energy consumption, so new processes must be developed to overcome the above shortcomings . Contents of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/025C07C29/04B01J8/06
Inventor 林立克杨高东周政张志炳
Owner NANJING ENETEKS
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