Environment-friendly process for producing dihydromyrcenol by using dihydromyrcene hydration reaction

A technology of dihydromyrcenol and dihydromyrcene, which is applied in the field of green technology, can solve the problems of low conversion rate and long reaction time, and achieves the effects of improving conversion rate, saving energy and equipment investment, and facilitating continuous operation.

Active Publication Date: 2010-03-31
厦门中坤化学有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the reaction time is usually long and the conversion rate is low

Method used

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  • Environment-friendly process for producing dihydromyrcenol by using dihydromyrcene hydration reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Dihydromyrcene, water and alcohol solvents (ethanol, propanol or butanol) are in a mass ratio of 1:1:1, preheated by preheaters 1, 2 and 3 respectively to reach a reaction temperature of 105°C and a pressure of 0.2 MPa (gauge pressure), and open the valve 27, with 10% sulfuric acid solution (addition is based on 100% H 2 SO 4 Calculated as accounting for 1% of the total material including solvent,) mixed into the jet reactor 5. The reaction material in the jet reactor 5 enters the ejector 8 in the jet reactor 5 through the outlet at the bottom of the jet reactor 5 through the centrifugal pump 9 and the heat exchanger 11 (the ejector is provided by Shuanghong Engineering Technology Development Co., Ltd. Provided, the same below.), sprayed into the jet reactor 5, and reacted. After the reaction was carried out for 3 hours, the valve 25 was opened, the jet reactor 5 began to discharge, and the reaction feed liquid entered the oil-water separator 7. Simultaneously, the r...

Embodiment 2

[0024] Similar to the operation process of Example 1, dihydromyrcene, water and acetone solvent are in a mass ratio of 1: 1: 2, respectively preheated through preheaters 1, 2 and 3 to reach a reaction temperature of 115 ° C, and a pressure of 0.5 MPa ( Gauge pressure), and open the valve 27, with 15% phosphoric acid solution (addition amount is based on 100% H 3 PO 4 Calculated as accounting for 1.2% of the total material including the solvent) mixed into the jet reactor 5. Other operating steps are the same as in Example 1. The conversion rate of dihydromyrcene in the process is over 98%, and the selectivity is over 92%.

Embodiment 3

[0026] Similar to the operation process of Example 1, dihydromyrcene, water and dioxane solvent are in a mass ratio of 1: 2: 2, and are preheated by preheaters 1, 2 and 3 respectively to reach a reaction temperature of 100° C. and a pressure of 0.1MPa (gauge pressure), and open valve 27, enter in jet reactor 5 after mixing with 15% p-toluenesulfonic acid (accounting for 100% p-toluenesulfonic acid is accounted for 15% including the total material of solvent). Other operating steps are the same as in Example 1. The conversion rate of dihydromyrcene in the process is over 90%, and the selectivity is over 90%.

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Abstract

The invention discloses an environment-friendly process for producing dihydromyrcenol by using a dihydromyrcene hydration reaction. The process adopts an integrated system consisting of a jet reaction device, an oil-water separation device and a rectification device. A high-speed injector is adopted in a reactor for reinforcing heat transfer and mass transfer of a reaction process; an acid (containing sulphuric acid, phosphoric acid and p-toluenesulfonic acid) is used as a catalyst and is in closed cycle; and an oil-water separator is arranged in the process flow to reduce the heat load of a rectification tower, and meanwhile the catalyst and the water phase in the oil-water separator are cycled and used in the system together so as to avoid the environment problems caused by the discharge of acid waste water. The process of the invention can improve the conversion rate of dihydromyrcene, and reduce the energy consumption and the production cost. Compared with a mechanical stirring reactor or a fixed bed reactor with the same scale, the process can improve the conversion rate of the dihydromyrcene by 1.2 to 4 times, and reduce the energy consumption of a dihydromyrcenol product per ton by more than 55 percent.

Description

field of invention [0001] The invention relates to a green process for producing dihydromyrcenol by hydration reaction of dihydromyrcene. technical background [0002] Dihydromyrcenol is an important fragrance with strong fruity, floral, green, woody and limey aromas, and the aroma has good stability in soaps and detergents. Dihydromyrcenol is generally synthesized by using dihydromyrcene and water as raw materials, and using sulfuric acid or other liquid acids or solid acids such as ion exchange resins as catalysts. Using liquid acid as a catalyst has strong acidity and high catalytic activity, but the reaction product generally needs to be neutralized and washed to remove sulfuric acid in the reaction product. The post-processing process is cumbersome, and waste discharge is easy to cause environmental pollution. Ion-exchange resins have high acid strength, are easy to separate, and can be reused, but have poor mechanical strength and high prices. The direct hydration r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/025C07C29/04B01J19/26B01D17/02B01J27/02B01J27/16B01J31/02
Inventor 张志炳周政刘勇傅华罗妮林力克杨毅融
Owner 厦门中坤化学有限公司
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