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Vacuum batch distillation process and device for purifying peach aldehyde from side discharge material

A technology of peach aldehyde and side stream, which is applied in the field of vacuum distillation separation and purification, can solve the problems of unqualified product purity, long operation time, high energy consumption, etc., achieve shortening of rectification process time, shorten rectification time, and improve rectification efficiency effect

Inactive Publication Date: 2015-05-06
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the intermittent rectification operation mode of tower top discharge takes a long time to operate, consumes a lot of energy, and has a low yield at one time. At the same time, there is a possibility that the purity of the product will not be qualified due to unclean removal of light components.

Method used

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  • Vacuum batch distillation process and device for purifying peach aldehyde from side discharge material
  • Vacuum batch distillation process and device for purifying peach aldehyde from side discharge material
  • Vacuum batch distillation process and device for purifying peach aldehyde from side discharge material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of device that carries out the vacuum space batch rectification process of purifying peach aldehyde by side discharge, as figure 1 As shown, it includes a rectification column tower kettle 2, a condenser 5, a reflux ratio controller 6, a side line discharge tower section 3, a vacuum pump and a collection tank 7, and the outside of the rectification tower is provided with a tower kettle heating jacket 1 and a condenser 5 It is connected to the top of the rectification tower, and the condenser 5 is connected to the rectification tower through a reflux pipeline. The reflux ratio controller 6 is set on the reflux pipeline. The inside of the rectification tower is provided with a packing layer 4, which is filled with high-efficiency separation Packing, high-efficiency separation packing is metal plate corrugated structured packing, wire mesh structured packing, metal mesh corrugated packing, grid packing, pulse packing or high-efficiency random packing. The tower body...

Embodiment 2

[0032] Add 437.3g peach aldehyde reaction crude product in tower still, the peach aldehyde content is 88% in the crude product. The rectification tower is filled with high-efficiency wire mesh structured packing, and the height of the tower is 1.2m.

[0033] Start the vacuum pump to evacuate the entire system. The jacket of the tower kettle is heated to 160°C, the tower body is kept at 80°C, and the condensing circulating water at the top of the tower is turned on. When there is reflux at the top of the tower, total reflux for 50 minutes, and the light components are slowly enriched at the top of the tower. When the temperature at the top of the tower is stable at about 92°C, 27g of octanol is extracted at a reflux ratio of 1:1, and then 30g of transition fraction is extracted by adjusting the reflux ratio to 4:1. Continue total reflux for 1 hour, the temperature at the top of the tower is stable at 95°C, and the temperature of the side line is stable at about 134°C. Start t...

Embodiment 3

[0036] Add 477.6g peach aldehyde reaction crude product in tower still, the peach aldehyde content is 88% in the crude product. The rectification tower is filled with high-efficiency wire mesh structured packing, and the height of the tower is 1.5m.

[0037]Start the vacuum pump to evacuate the entire system. The jacket of the tower kettle is heated to 160°C, the tower body is kept at 80°C, and the condensing circulating water at the top of the tower is turned on. When there is reflux at the top of the tower, total reflux for 50 minutes, and the light components are slowly enriched at the top of the tower. When the temperature at the top of the tower is stable at around 90°C, 29g of octanol is extracted at a reflux ratio of 1:1, and then 30g of transition fraction is extracted by adjusting the reflux ratio to 4:1. Continue the total reflux for 1 hour, the temperature at the top of the tower is stable at 93°C, and the temperature of the side line is stable at about 133°C. Sta...

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Abstract

The invention relates to a vacuum batch distillation process and device for purifying peach aldehyde from a side discharge material. The vacuum batch distillation process comprises the following steps: adding a crude peach aldehyde product into a distilling column bottom at one time; vacuuming a distilling column; heating the column bottom to be 140-160 DEG C; keeping the column body at 50-80 DEG C; opening the column top to condense circulation water; when the column top has a reflux liquid, slowly enriching light components on the column top; when the temperature of the column top is stabilized to be 86-95 DEG C, acquiring 8-12wt% of capryl alcohol and transition fraction according to a variable reflux ratio; continuously implementing total reflux, and acquiring a peach aldehyde product from a low-level side discharge point when keeping the temperature of the column top at 85-95 DEG C and the temperature of a side at 120-140 DEG C; continuously implementing total reflux, rising the side acquiring position, and acquiring a residual peach aldehyde product from a high-level side discharge point. Compared with the prior art, on the basis of vacuum distillation, the vacuum batch distillation process adopts a vacuum side material discharge method, so that the yield of peach aldehyde is greatly increased, the distillation time is shortened, the energy consumption is reduced, the distillation efficiency is improved, and the purity of the product is greater than that of a column top discharge material.

Description

technical field [0001] The invention relates to vacuum rectification separation and purification technology, in particular to a vacuum batch rectification process and device for purifying peach aldehyde by side line discharge. Background technique [0002] Peach aldehyde, also known as α-heptyl-γ-butyrolactone, is a colorless, transparent to slightly yellow liquid with a strong peach aroma. Extract Manufacturers Association) identified as GRAS (Generally Recognized as Safe), approved by the FDA (Food and Drug Administration), and included in the list of artificial food flavors that can be used in food without endangering human health by the European Council . It is often used in daily spices such as osmanthus, jasmine, gardenia, lily of the valley, orange blossom, white rose, lilac, golden lily, etc. It is also a good choice for food flavors such as peaches, melons, plums, apricots, cherries, and osmanthus raw material. Almost insoluble in water, soluble in ethanol and mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01D3/10B01D3/14B01D3/42
CPCC07D307/33B01D3/10B01D3/14B01D3/42
Inventor 艾波翟金国许保云李良君张丽雅包春凤吴高胜江孝平束世平
Owner SHANGHAI RES INST OF CHEM IND
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