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Acraldehyde recovering method

A recovery method and acrolein technology, applied in the separation/purification of carbonyl compounds, etc., can solve the problems of affecting the life of the hydrogenation catalyst, difficult to reduce the content of acrolein, and unsuitable for separation of acrolein, etc.

Inactive Publication Date: 2004-11-17
HEILONGJIANG INST OF PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, the acrolein hydration reaction is carried out under the action of an acidic catalyst. The reaction is a reversible reaction. The 3-hydroxypropionaldehyde aqueous solution produced contains about 2-10% unreacted acrolein by weight. If this part of acrolein is not added Recovery will form a variety of by-products in the next hydrogenation reaction of 3-hydroxypropionaldehyde, which will rapidly reduce the activity of the hydrogenation catalyst, affect the life of the hydrogenation catalyst, and increase the consumption quota
With the distillation of acrolein, 3-hydroxypropanal will decompose into acrolein and water, and 3-hydroxypropanal is very unstable, and it is easy to undergo polymerization and condensation reactions by itself or with acrolein under heated conditions, resulting in The content of acrolein in the 3-hydroxypropanal hydration solution is difficult to reduce to meet the requirements of hydrogenation, and the separated liquid is not suitable as a raw material for hydrogenation because it contains high polymers, so the existing methods are not suitable for separating acrolein in the aqueous solution of 3-hydroxypropanal acrolein
U.S. Patents US3518310, US5015789, US5093537, and US6140543 all mentioned the use of a thin-film evaporator to separate acrolein in the 3-hydroxypropionaldehyde hydration solution, and shorten the contact time between the hydration solution and the heat source as much as possible to avoid side reactions. The recovery rate of aldehyde has been improved, but the investment of thin-film evaporator equipment required is large, and the operation is also relatively difficult

Method used

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specific Embodiment approach 1

[0005] Specific embodiment one: In this embodiment, the 3-hydroxy propionaldehyde aqueous solution containing 2.9% by weight of acrolein in the acrolein hydration reaction is passed into the raw material tank 1, and the vacuum pump 11 is turned on to make the rectification tower 4 vacuum, and the 3- The aqueous solution of hydroxypropionaldehyde enters the preheater 3 after being measured by the flowmeter 2, and the temperature of the material entering the middle part of the rectification tower 4 after preheating is 55~58°C, so that the superficial liquid velocity of the aqueous solution of 3-hydroxypropionaldehyde is 0.5m / h, the number of trays in the rectifying tower 4 is 17 to 21, the vacuum degree of the rectifying tower 4 is -0.076 to -0.080Mpa, and the air preheated to 55 to 58°C is introduced, the gas-liquid volume ratio The ratio is 10 to 12 times, and the weight content of acrolein in the aqueous solution of 3-hydroxy propionaldehyde after separation is reduced from 2....

specific Embodiment approach 2

[0006] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is that the 3-hydroxy propionaldehyde aqueous solution containing 3.5% by weight of acrolein in the acrolein hydration reaction is passed into the raw material tank 1, and then enters the middle material of the rectification tower 4 The temperature is 58~62℃, the superficial liquid velocity is 0.6m / h, the number of trays of the rectifying tower 4 is 12~16, and the vacuum degree of the rectifying tower 4 is -0.084~-0.086Mpa. The air heated to 58-62°C has a gas-liquid volume ratio of 14-16 times. After separation, the weight content of acrolein in the 3-hydroxy propionaldehyde aqueous solution is reduced from 3.5% to 0.8%. Its recycling process is the same as the specific embodiment one.

specific Embodiment approach 3

[0007] Specific embodiment 3: This embodiment is different from specific embodiment 1 in that the 3-hydroxypropionaldehyde aqueous solution containing 6.1% by weight of acrolein in the acrolein hydration reaction is passed into the raw material tank 1, and then enters the middle material of the rectification tower 4 The temperature is 62~65℃, the superficial liquid velocity is 0.6m / h, the number of trays of the rectifying tower 4 is 12~16, the vacuum degree is -0.082~-0.084Mpa, and it is preheated to 62~65 In the air at ℃, the gas-liquid volume ratio is 14-16 times. After separation, the weight content of acrolein in the 3-hydroxy propionaldehyde aqueous solution is reduced from 6.1% to 0.8%. Its recycling process is the same as the specific embodiment one.

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Abstract

The present invention is a method of separating and recovering unreacted acraldehyde from the reacted liquid of hydrolyzing acraldehyde to prepare 3-hydroxy propionic aldehyde. The recovering process includes preheating an aqueous solution of 3-hydroxy propionic aldehyde with 2-10 wt% of acraldehyde to 50-75 deg.C; and treating in the middle part of a refining tower under the solution speed of 0.1-2.0 m / hr and vacuum degree of 0.066-0.092 MPa while introducing inert gas of 5-25 times the volume of the aqueous solution and heated to 50-75 deg.C from the bottom of the tower; cooling the distrilled liquid from the top of the tower to obtain the aqueous, solution of rich acraldehyde content. The said method can reduce the consumption of acraldehyde and prolong the service life of the catalyst.

Description

Technical field: [0001] The invention relates to a method for separating and recovering unreacted acrolein from the reaction liquid produced in the reaction process of preparing 3-hydroxypropanal by hydration of acrolein. Background technique: [0002] At present, the recovery of acrolein basically adopts traditional fractionation and rectification methods. Due to the active chemical properties of acrolein and 3-hydroxypropanal, the recovery rate is very low. Generally, the acrolein hydration reaction is carried out under the action of an acidic catalyst. The reaction is a reversible reaction. The 3-hydroxypropionaldehyde aqueous solution produced contains about 2-10% unreacted acrolein by weight. If this part of acrolein is not added Recycling will form a variety of by-products in the next step of 3-hydroxypropanal hydrogenation reaction, which will rapidly reduce the activity of the hydrogenation catalyst, affect the life of the hydrogenation catalyst, and increase the con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/82C07C47/22
Inventor 白雪峰李猛韩大维
Owner HEILONGJIANG INST OF PETROCHEM
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