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Method for separating and recycling acetaldehyde

A technology for separation and recovery of acetaldehyde, applied in the direction of organic chemistry, etc., can solve problems affecting the yield and quality of glyoxal, reducing fluidity, and coloring of products, so as to save energy and auxiliary materials, improve quality, and reduce The effect of production costs

Inactive Publication Date: 2013-08-07
严恒系 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, acetaldehyde recovery adopts rectification process, but because glyoxal is extremely active, it is easy to react with aldehydes, etc., and irreversible polymerization will occur when overheating, which will cause coloring of the product, and glue will be formed during deep polymerization. solids, seriously affecting the yield and quality of the product glyoxal, increasing viscosity and reducing fluidity, which brings great difficulties to follow-up processing

Method used

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  • Method for separating and recycling acetaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Preheating of liquid to be treated→air stripping

[0023] Place the 500mL three-necked bottle in a constant temperature water bath and install a stirrer. figure 1 for

[0024] Add the solution to be treated (referring to the mixed aqueous solution of acetaldehyde, glyoxal, nitric acid and acetic acid in the process of preparing glyoxal by acetaldehyde nitric acid oxidation) into the three-necked bottle, and when the temperature reaches 30-40°C, start stirring, and at the same time Continuously feed nitrogen into the bottle at a gas flow rate of 15L / min;

[0025] After 2.8 hours, the content of acetaldehyde in the feed liquid decreased from 4.38% to 0.23%, and the main amount of acetaldehyde was discharged with nitrogen, collectively called the mixed gas A1 of nitrogen and acetaldehyde.

Embodiment 2

[0026] Example 2 Preheating of liquid to be treated→air stripping

[0027] The inner diameter of the packed tower is 20mm, the packing height is 800mm, and the packing is a glass silk ring. In the process, the mixed aqueous solution of acetaldehyde, glyoxal, nitric acid and acetic acid) is continuously added from the top of the tower.

[0028] The electric heating belt voltage is 40V, the temperature in the middle of the tower is 40°C, the liquid volume at the top of the tower is 60mL / min, and the gas volume is 15L / min.

[0029] The composition of feed liquid entering the tower is 3.94% of acetaldehyde, 10.06% of glyoxal, 3.55% of nitric acid and 5.83% of acetic acid.

[0030] The feed liquid from the tower kettle consists of 0.27% acetaldehyde, 11.09% glyoxal, 3.50% nitric acid, and 6.46% acetic acid; the main amount of acetaldehyde is discharged with nitrogen, which is collectively called the mixed gas A2 of nitrogen and acetaldehyde.

Embodiment 3

[0031] Example 3 Absorption—Absorb the mixed gas A2 obtained by stripping with a solvent

[0032] The inner diameter of the packed tower is 20mm, the packing height is 1800mm, the packing is glass fiber ring, and the tower is vacuum jacketed.

[0033] The mixed gas A2 of nitrogen and acetaldehyde is continuously fed into the bottom of the tower. The gas is absorbed by primary water spraying, and the flow rate of the absorbed water is controlled by a micro rotor flowmeter. The absorbed water is cooled to below 10°C by the refrigerator, and continuously sprayed into the tower , to obtain dilute acetaldehyde solution B1, the concentration is 5.92%, the acidity of dilute acetaldehyde (calculated as acetic acid, the same below) is 0.09%; the content of acetaldehyde in the exhaust tail gas is 0.08%.

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Abstract

The invention discloses a method for separating and recovering acetaldehyde, which includes the steps of preheating, gas stripping and absorption. Blow out, the acetaldehyde-containing gas is absorbed through the absorption tower spraying solvent in multiple stages to obtain a dilute solution, and then concentrated under reduced pressure to obtain concentrated acetaldehyde. The method has a high yield of acetaldehyde, and avoids the problem of discoloration of products existing in direct distillation in the prior art, and at the same time avoids environmental pollution caused by decolorization using activated carbon, saves energy and auxiliary materials, and reduces production costs. The invention is suitable for the separation and recovery system of the acetaldehyde in the reaction solution when the acetaldehyde is used as the starting material to prepare the glyoxal by nitric acid oxidation, and can be widely used in the recovery and separation of low-boiling point materials in other heat-sensitive materials.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to the recovery of acetaldehyde in the process of preparing glyoxal by nitric acid oxidation with acetaldehyde as a starting material, in particular to a method for separating and recovering acetaldehyde. Background technique [0002] The preparation methods of glyoxal include ethylene oxidation method, acetylene oxidation method, oxalic acid reduction hydrolysis method, ethylene glycol gas phase oxidation method, acetaldehyde nitric acid oxidation method, etc. Among them, ethylene glycol gas phase oxidation method and acetaldehyde nitric acid oxidation method The method is the most commonly used in the world, and the production capacity of the two methods is equivalent, while the other methods are not often used due to immature technology, high raw material consumption, and serious pollution. [0003] The process of producing glyoxal by nitric acid oxidation of acetaldehyde has the c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/09
Inventor 赵地顺扈士海李雪刚李银江张拴力王翠丽刘进展张会娟张志华王占强闫峰光
Owner 严恒系