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Complexing agent adding depression batch fractionating process for purifying linalyl acetate

A technology of linalyl acetate and complexing agent, which is applied in the process field of purifying linalyl acetate by vacuum batch distillation with complexing agent added, can solve the problems of complicated process, troublesome condensation-cooling, etc., and reduce the temperature of the kettle , less energy consumption and high product purity

Inactive Publication Date: 2005-11-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The separation method of existing heat-sensitive substances mainly adopts vacuum rectification, or feeds inert gas or water vapor to reduce the partial pressure, to lower the temperature of the kettle, and avoid the heat-sensitive substances from reacting or decomposing and deteriorating due to overheating. Cooling is troublesome and complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Separate and purify linalyl acetate with a vacuum batch rectification tower. The inner diameter of the rectification tower is Φ50mm, and a 20mm×20mmθ ring stainless steel wire mesh packing is installed inside, and the filling height of the packing is 1m. Add linalyl acetate crude product 440g, wherein contain linalyl acetate 53% (mass fraction, the same below), light impurity component 29%, also have heavy impurity component 11%; Add sodium chloride 3g. In the rectification operation, when the temperature of the bottom of the tower is 98°C-100°C and the temperature of the top of the tower is 35°C-38°C, 184g of light impurity components are extracted from the top of the tower with a reflux ratio of 10 / 1-5 / 1; The temperature of the kettle is 110°C-115°C, the temperature of the tower top is 50°C-54°C, the pressure of the tower top is 1.5KPa, the pressure drop of the whole tower is 2.4KPa, the preheating is 1h, the total reflux is 1h, and the constant reflux ratio is 1 (or ...

Embodiment 2

[0012] Adopt the rectifying device identical with embodiment 1, fill 1 meter of 10mm * 10mm porcelain Raschig ring fillers, other implementation conditions are identical with embodiment 1. In the rectification operation, when the still temperature is 100°C-102°C and the top temperature is 40°C-45°C, 160g of light impurity components are extracted from the top of the tower at a reflux ratio of 10 / 1-5 / 1; the still temperature is 115 ℃-118℃, top temperature 52℃-54℃, tower top pressure 1.4KPa, total tower pressure drop 2.5KPa, preheating for 1h, full reflux for 2h, operating with a reflux ratio of 2 / 1-1 / 1; Obtain 220 g of linalyl acetate with a purity greater than 95% from the top of the tower, with a yield of 70%; 40 g of still liquid remains; the operation cycle is 9 hours long.

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PUM

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Abstract

The invention discloses a process for purifying linalyl acetate through decompression batch fractionating for complexing agent addition, wherein vacuum rectification tower filled by highly effective theta ring padding is employed to prepare linalyl acetate with pureness greater than 95% from the coarse product of linalyl acetate, characterized in that, 0.5%-1% of sodium chloride, or calcium chloride, potassium chloride is charged by the weight ratio of the raw material, the operational condition of the tower being, the tower still temperature 98 deg. C -118 deg. C, the tower top temperature 35 deg. C -54 deg. C, the tower top operating pressure 1.4 KPa to 1.5 KPa, the variable reflux ratio of 10 / 1-1 / 1 is adopted to prepare light impure components and linalyl acetate product.

Description

technical field [0001] The invention relates to a separation process of heat-sensitive spices, in particular to a separation method of heat-sensitive substances containing linalyl acid. Background technique [0002] Linalyl acetate (chemical name is 3,7-dimethyl-1,6-octadien-3-ol acetate) is an indispensable spice for the preparation of high-grade flavors, and occupies an important position in the daily chemical, tobacco, and food industries. very important position. It has an elegant aroma similar to essential oils such as lily of the valley and lavender, and is widely used in the preparation of soap essence, perfume essence, cosmetic essence, food essence, etc. [0003] With the increasing demand for daily cosmetics and their high-end products, the demand for linalyl acetate will increase greatly, so the research on the synthesis method of linalyl acetate and the improvement of product yield is of great significance. At present, linalyl acetate can be obtained in the syn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/54C07C69/145
Inventor 韩金玉张海英常贺英王华李凭力魏文英
Owner TIANJIN UNIV