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System for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification

A side-line and material-refining technology, applied in fractionation, organic chemistry, etc., can solve the problems of poor aroma, large loss of peach aldehyde, and low primary yield.

Active Publication Date: 2015-07-22
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because peach aldehyde is the intermediate component in the synthetic crude product, tower top will obtain high-purity peach aldehyde, first step tower top first extracts octanol, the second step extracts transition fraction, the third step extracts reworked product, this The mass fraction of peach aldehyde contained in the reworked product extracted at the time is close to the finished product, resulting in a large loss of peach aldehyde, resulting in a low yield of the entire process at the end, and the obtained peach aldehyde product always contains a small amount of light components Impurities, poor product aroma
Patent CN202246491U introduces a set of peach aldehyde rectification equipment, which mainly solves the separation of peach aldehyde and requires two sets of equipment with different structures, that is, a flash device and a rectification device. High consumption, low yield, long time consumption, and low product purity and poor aroma

Method used

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  • System for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification
  • System for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a rectification tower with a height of 12 meters and a diameter of 500mm, the opening area of ​​the liquid collector is 40%, the length of the riser pipe is 100mm, and the distribution points of the liquid distributor are 208 per square meter, through the feed centrifugal pump And the feed regulating valve puts 2000kg crude peach aldehyde into the tower kettle, the content of peach aldehyde in the crude product is 88.08%, of which the content of impurities lower than the boiling point of peach aldehyde is 8.31%, and the content of impurities higher than the boiling point of peach aldehyde is 3.61%, and then start Cooling water system, start the vacuum pump group, when the system reaches the required pressure for separation, when the absolute pressure is equal to 1kPa, start the material circulation centrifugal pump and adjust the flow to 2.5m 3 / h, the material is circulated in the tower kettle and the falling film reboiler through the circulating material-liquid regula...

Embodiment 2

[0024] The operation steps are the same as in Example 1, adjust the circulating flow to 1m 3 / h, the heat transfer oil temperature is 220℃. The analysis results proved that the content of peach aldehyde in the product reached 99.23%, and the yield was 86%. figure 2 In order to collect the gas chromatogram of the product, it can be seen from the figure that there is no impurity peak in front of the peach aldehyde peak, which means that there is no light component in the sample. There are two small impurity peaks behind the peach aldehyde peak, but the content is very low, and the heavy components have little effect on the aroma of peach aldehyde. The peach aldehyde product with such a content can be obtained because there are basically no light components in the side line discharge position, and the peach aldehyde content is relatively high.

Embodiment 3

[0026] The operation steps are the same as in Example 1, adjust the circulating flow to 4m 3 / h, the heat transfer oil temperature is 240℃. The analysis results proved that the content of peach aldehyde in the product reached 98.71%, and the yield was 81.35%.

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Abstract

The invention relates to a system for purifying peach aldehyde through decompressed intermittent side withdrawal and rectification. The system comprises a tower kettle, a main tower and a condenser, which are connected in sequence from the bottom to top, wherein the side part of the main tower is connected with a side withdrawal device; the tower top of the main tower is connected with a tower top discharging device; the whole system is connected with a vacuum pump group through a buffer tank; through the vacuum pump group, the absolute pressure is not greater than 1 kPa. Compared with the prior art, the system provided by the invention is capable of solving the problems that the micro impurity components in the product are difficult to remove in the industrial peach aldehyde separation and the product is bad in fragrance, long in rectification time, low in yield and large in energy consumption, and a rectification device for producing high-quality peach aldehyde is provided; according to the device, tower top separation is carried out to extract the light components in the raw materials and side extraction is carried out to obtain high-quality peach aldehyde products; the device is flexible to operate, short in rectification operation time and high in production efficiency; the peach aldehyde yield is within 82-85%, the purity of the peach aldehyde product is 99.2% or above and the product does not contain light components which influence the fragrance.

Description

Technical field [0001] The invention relates to a peach aldehyde separation technology, in particular to a system for purifying peach aldehyde by rectifying and purifying peach aldehyde with intermittent side-line discharge under reduced pressure. Background technique [0002] Peach aldehyde, also known as α-heptyl- -Butyrolactone, myristaldehyde, is a colorless, transparent to slightly yellow liquid with a strong peach aroma. As one of the most commonly used lactone flavors, it is recognized by FEMA (American Flavor and Extract Manufacturers Association) It is GRAS (generally recognized as safe), FEMA number 3091, and approved by the FDA (U.S. Food and Drug Administration) for consumption. The European Council has listed peach aldehyde in the list of artificial flavors that can be used in food without harming human health. Peach aldehyde is commonly used in daily spices such as osmanthus, jasmine, gardenia, lily of the valley, orange blossom, white rose, lilac, golden lily, etc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D3/14C07D307/33
Inventor 江孝平许保云吴高胜艾波包春凤翟金国李良君束世平
Owner SHANGHAI RES INST OF CHEM IND