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Dihydromyrcenol fixed bed hydration continuous production method

A technology of dihydromyrcenol and dihydromyrcene, which is applied in the field of continuous production of dihydromyrcenol fixed bed hydration to achieve the effects of reduced breakage rate, small volume and increased loss

Active Publication Date: 2013-11-20
JIANGSU XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] First of all, a unique U-bend reactor is adopted, and the catalyst is loaded from the upper end. When replacing, open the discharge port at the lower end to discharge, which effectively solves the problem of catalyst replacement in the catalyst bed reactor.

Method used

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  • Dihydromyrcenol fixed bed hydration continuous production method

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Effect test

Embodiment 1

[0029] Fill the solid acid catalyst in the tubular reactor 4 in advance, use the ion exchange resin as the solid acid catalyst, the ion exchange resin in this place is the conventional ion exchange resin on the market (such as: macroporous strongly acidic styrene series cation exchange resin, etc.). Dihydromyrcene, solvent (dioxane): water, according to the mass ratio of 1:1:1, are preheated by feed preheaters 1 and 2 respectively to reach a reaction temperature of 80°C, and then pass through a pressurized injection device 3 After homogenization, it enters the tubular reactor 4 for reaction. After the liquid is filled with the tubular reactor 4, it enters the oil-water separator 5 through the catalyst filter 17 for oil-water layering. The lower water layer is returned to the solvent aqueous solution tank through the centrifugal pump 18, and the oil layer Enter the rectification tower 10 through the centrifugal pump 6 and the feed preheater 7. After being separated by the recti...

Embodiment 2

[0032] Dihydromyrcene, solvent acetone: water, according to the ratio of mass ratio 1: 0.5: 0.5, reach 70 ℃ of reaction temperature through the preheating of feed preheater 1,2 respectively, other conditions are with embodiment 1, the second step of this process The conversion rate of hydromyrcene is 91.5%, and the selectivity is over 92%.

Embodiment 3

[0034] Similar to the operation process of Example 1, pure water replaces the solvent aqueous solution to participate in the reaction, and is preheated by feed preheaters 1 and 2 respectively to reach a reaction temperature of 75°C. The conversion rate of dihydromyrcene in this process is more than 85%. Sex is above 93%.

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Abstract

The invention discloses a production method of spice and in particular relates to a dihydromyrcenol fixed bed hydration continuous production method. The method comprises the following steps of: allowing dihydromyrcene, water or aqueous solution of a solvent to enter a feeding preheater respectively through a head tank and a flowmeter to perform preheating; allowing the reaction materials to enter a tubular reactor continuously and then overflow into an oil water separator to be separated; and allowing the lower layer aqueous phase to enter a reaction system continuously and circularly and allowing the oil layer to enter a rectifying tower to perform rectification, wherein the tower is provided with three discharge ports; and materials of different concentrations are discharged from the discharge ports respectively. The method has the advantages of really realizing zero emission of waste water, making the using ratio of pure water close to 100 percent, saving cost of raw materials, exchanging catalysts conveniently and simply, greatly prolonging the service life of the catalysts, solving the problem of escape of the catalysts, expanding easily, fulfilling the aim of zero use of the solvent and saving solvent cost, along with low equipment investment and wide application.

Description

field of invention [0001] The invention relates to a production method of spices, in particular to a continuous production method of dihydromyrcenol fixed bed hydration. technical background [0002] Dihydromyrcenol has a wide range of uses and is one of the important fragrance raw materials today. It has green, sweet, powerful, fresh citrus, cypress, lavender, fruity, floral, white lemon, and cologne. The aroma is used in soaps and detergents. has good stability. Nowadays, it is often one of the raw materials used in excess in new fragrance formulations. Dihydromyrcenol is generally synthesized by using dihydromyrcene and water as raw materials, and using sulfuric acid or other liquid acids or ion catalysts as catalysts. The use of liquid acid as a catalyst has the advantages of strong acidity and high catalytic activity, but the reaction product contains high acidity, and the material must be processed by neutralization and water washing, and waste discharge will cause e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/025C07C29/04C07C29/80
Inventor 陈绣芳包江峰王卫明应登宇谢自强兰昭洪李道权
Owner JIANGSU XINHUA CHEM
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