Method for continuously producing dihydromyrcenol by using tubular reactor

A tubular reactor and dihydromyrcenol technology, applied in organic chemistry, hydroxyl addition preparation, etc., can solve the problems of rapid decline in reaction rate, high process energy consumption, low production efficiency, etc., to save equipment investment, The effect of large heat transfer area and high production capacity

Inactive Publication Date: 2012-09-12
淮安市产品质量监督检验所
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the disadvantages of high energy consumption, low production efficiency and serious environmental pollution in the existing process, the present invention provides a method for continuous production of dihydromyrcenol with a tubular reactor, which uses a tubular reactor instead of a batch stirred tank reactor , reduce liqui...

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  • Method for continuously producing dihydromyrcenol by using tubular reactor
  • Method for continuously producing dihydromyrcenol by using tubular reactor

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Embodiment 1

[0020] Example 1: The mass ratio of dihydromyrcene, water, and isopropanol is 1:1:1, preheated to 80°C after being mixed by a mixer o C, enter the tubular reactor; add Amberlyst 36 strong acid type macroporous cation exchange resin as catalyst in the tubular reactor, the tubular reactor adopts short-circuit current heating, control reaction temperature 110 o C. After the reaction product is filtered through the screen at the outlet of the tubular reactor, the catalyst is retained in the reactor for continued use, and the filtrate enters the phase separator; after the filtrate is separated by the phase separator, the water phase is pumped into the mixer as a raw material Recycling, the upper organic phase enters the rectification tower for further separation; the mixture of dihydromyrcene and solvent extracted from the top of the rectification tower is sent to the mixer as a raw material for continued use, and the product dihydromyrcenol is extracted from the tower reactor, with...

Embodiment 2

[0021] Example 2: Similar to the operation method of Example 1, the mass ratio of dihydromyrcene, water, and butanol is 1:2:2, and it is preheated to 90°C after being mixed by a mixer. o C, enter the tubular reactor; add a certain amount of Amberlyst 15 strong acid type macroporous cation exchange resin in the tubular reactor, control the reaction temperature 100 o C, other operation steps are the same as embodiment 1, and the purity of dihydromyrcenol in the tower kettle is 95.6%. The conversion rate of dihydromyrcene was 94%, and the selectivity was 91%.

Embodiment 3

[0022] Embodiment 3: Similar to the operation method of Embodiment 1, the mass ratio of dihydromyrcene, water and methanol is 1:3:3, preheated to 85 o C, add a certain amount of Amberlyst 35 strong acid type macroporous cation exchange resin in the tubular reactor, control reaction temperature 120 o C, other operation steps are the same as embodiment 1, and the purity of dihydromyrcenol in the tower kettle is 96%. The conversion rate of dihydromyrcene is 90%, and the selectivity is 92%.

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Abstract

The invention discloses a method for continuously producing dihydromyrcenol by using a tubular reactor. The method comprises the following steps: mixing dihydromyrcene, water and solvent in a mixer; after mixing, heating the mixture to 70-95 DEG C by a pre-heater and pouring the mixture into the tubular reactor; heating and controlling the reaction temperature in the tubular reactor at 100-120 DEG C by adopting a short circuit current; pouring a reaction product in the tubular reactor into a phase splitter; after splitting the phases by the phase splitter, further separating the upper-layer organic phase in a rectifying column; pouring the upper-layer organic phase into the rectifying column after splitting the phases by the phase splitter, causing the dihydromyrcenol as a heavy component to flow to a tower kettle; and extracting the dihydromyrcenol with purity above 95% by the tower kettle. The tubular reactor is adopted according to the method provided by the invention, for reducing liquid back-mixing, reducing energy consumption and avoiding the quick decrease of reaction rate in the later stage of reaction. A fin is arranged on the inner wall of the tubular reactor, for reinforcing the liquid flow, boosting the matter-transferring and heat-transferring of reaction, increasing the reaction rate and meanwhile avoiding the powdering of solid catalyst caused by stirring.

Description

technical field [0001] The invention relates to a production method, in particular to a method for continuous production of dihydromyrcenol by a tubular reactor. Background technique [0002] Dihydromyrcenol (2,6-dimethyl-7-octen-2-ol) is a commonly used and important terpenoid spice, and it is one of the most widely used spices in the world. It has a fresh floral and lemon-like fruity aroma. It is used in lime and citrus daily essences. It can be used in soaps and detergents at a dosage of 5% to 20%. It is "excessively used" in modern men's perfumes representative. At present, there are two main methods for producing dihydromyrcenol: indirect hydration method and direct hydration method. Industrial production mainly uses concentrated H 2 SO 4 It is used as a catalyst for indirect hydration of dihydromyrcene and formic esterification and saponification. The conversion rate and selectivity of this method are low, the energy consumption is large, and concentrated H 2 SO ...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/04
Inventor 陈长毅陈枚熊金龙夏珊珊
Owner 淮安市产品质量监督检验所
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