Method for preparing dihydromyrcenol through reaction distillation continuity

A technology for dihydromyrcenol and dihydromyrcene is applied in the field of continuous preparation of dihydromyrcenol by reactive distillation, which can solve the problems of high investment cost, complicated process, low integration and the like, and achieves the reduction of environmental pollution, The effect of improving the conversion rate and simplifying the production process

Inactive Publication Date: 2012-08-01
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 shortcomings of the existing process flow complex, low integration, high investment cost and serious environmental pollution, the purpose of the present invention is to provide a continuous Process for chemically producing dihydromyrcenol

Method used

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  • Method for preparing dihydromyrcenol through reaction distillation continuity
  • Method for preparing dihydromyrcenol through reaction distillation continuity
  • Method for preparing dihydromyrcenol through reaction distillation continuity

Examples

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Effect test

Embodiment 2

[0025] The operation method is the same as that of Example 1. Before starting work, add dihydromyrcene, water, isopropanol (or butanol or acetate) in a mass ratio of 1:(1~3):(1~3) into the reaction mixture. Distillation tower 7, adding Amberlyst 35 strong acid type macroporous cation exchange resin. The catalyst in the reaction section of the reactive distillation tower is Amberlyst 35 strong acid macroporous cation exchange resin, and dihydromyrcene, water and isopropanol are preheated to 102℃, 93℃ and 75℃ respectively. Other operation steps are the same as in Example 1. The purity of the bottom dihydromyrcenol is 96%. The conversion rate of dihydromyrcene was 95%, and the selectivity was 93%.

Embodiment 3

[0027] Similar to the operation method of Example 1, add dihydromyrcene, water and isopropanol to the tower kettle in a mass ratio of 1:1:1 to 1:3:3, and add a certain amount of Amberlyst 15 strong acid type macroporous cation exchange resin . The catalyst in the reaction section of the reactive distillation tower is Amberlyst 15 strong acid type macroporous cation exchange resin. Dihydromyrcene, water and isopropanol are preheated to 100℃, 80℃ and 78℃ respectively. Other operation steps are the same as in Example 1. The purity of the bottom dihydromyrcenol is 95%. The conversion rate of dihydromyrcene was 95%, and the selectivity was 91%.

Embodiment 4

[0029] Similar to the operation method of Example 1, the catalyst adopts Purilite CT275 strong acid type macroporous cation exchange resin, and dihydromyrcene, water and dioxane are preheated to 93°C, 87°C and 70°C, respectively. Other operation steps are the same as in Example 1. The purity of the bottom dihydromyrcenol is 95%. The conversion rate of dihydromyrcene was 95%, and the selectivity was 93%.

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Abstract

The invention relates to a method for preparing dihydromyrcenol through reaction distillation continuity. Corrugated gauze filling materials and solid acid catalysts are filled in a reaction distillation tower, raw materials of dihydromyrcene, water and solvents are respectively preheated to 80 to 120 DEG C, 85 to 95 DEG C and 70 to 90 DEG C to be respectively fed from the upper part, the middle part and the lower part of a reaction section of the reaction distillation tower according to the flow rate ratio of (1-3): (1-3). The tower kettle temperature is controlled to be 105 to 120 DEG C, and the tower top condensing temperature is controlled to be 50 to 70 DEG C. An oil phase and a water phase are separated out from condensed liquid, partial oil phase reaches the tower top to flow back, and the water phase and the rest oil phase respectively return a raw material tank to be cyclically utilized. According to the method, the reaction and the distillation are simultaneously carried out, heat released by the reaction can be effectively utilized for heating materials, and a heat load of a tower kettle is reduced. The corrugated gauze filling materials in the reaction distillation tower and a tubular liquid distributor are favorable for improving the effective surfaces for mass transfer and heat transfer and improving the inter phase contact, dihydromyrcenol products with the purity being 95 percent are obtained from the tower bottom, and the reaction efficiency and the dihydromyrcenol conversion rate are higher.

Description

Technical field [0001] The invention relates to a method for preparing dihydromyrcenol, in particular to a method for continuously preparing dihydromyrcenol by reactive distillation. Background technique [0002] Dihydromyrcenol (2,6-dimethyl-7-octene-2-ol) is a commonly used important terpenoid fragrance and one of the most used fragrance varieties in the world. It has a fresh floral fragrance and a white lemon-like fruity fragrance. It is used in white lemon and citrus-type daily flavors. The amount used in soaps and detergents can reach 5%-20%. The current methods for producing dihydromyrcenol mainly include indirect hydration and direct hydration. Industrial production mainly uses concentrated H 2 SO 4 As a catalyst, the indirect hydration method of dihydromyrcene and formate and saponification; this method has low conversion rate and selectivity, and concentrated H 2 SO 4 The equipment is severely corroded, and the discharged wastewater can easily cause environmental pollut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/025C07C29/04C07C29/80
CPCY02P20/10
Inventor 陈玉波夏珊珊牛雁宁
Owner 淮安市产品质量监督检验所
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