Preparation method of acetaldoxime

An acetaldoxime and reaction technology, which is applied in the field of preparation of acetaldoxime, can solve the problems of waste acid discharge in wastewater, large amount of hydroxylamine salt, long reaction process, etc., and achieves high adsorption efficiency, short reaction process and good adsorption effect. Effect

Inactive Publication Date: 2020-05-08
ZHEJIANG JINHUA NEW MATERIALS
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above invention and the method for preparing acetaldehyde to synthesize acetaldehyde oxime in the prior art is to synthesize acetaldehyde oxime with acetaldehyde and hydroxylamine sulfate. The consumption is large, and a large amount of low-value ammonium sulfate is produced as a by-product, which is difficult to handle and high in cost. At the same time, toxic substances such as sulfur dioxide and sodium nitrite are used, and waste water and waste acid containing sodium sulfate and ammonium sulfate are discharged, which is not good for the environment.

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  • Preparation method of acetaldoxime
  • Preparation method of acetaldoxime

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Effect test

Embodiment 1

[0025] A kind of preparation method of acetaldehyde oxime, its operation step is:

[0026] According to the number of parts by mass, 40-Kg hydroxylamine phosphate, 8.4Kg acetaldehyde and 260Kg water were added to the reactor, the temperature was controlled at 30°C, and the reaction mixture was obtained after 2 hours of reaction; the reaction mixture entered the stripping tower, and the organic matter and part Water is steamed from the top of the tower, and the purified inorganic liquid at the bottom of the tower is returned to the front system for recycling to make hydroxylamine phosphate; while the top liquid of the stripping tower enters the rectification system for separation and purification, and finally obtains a 47% acetaldehyde oxime aqueous solution Product; it is characterized in that described purification operation adopts a kind of graphene modified adsorbent packing adsorption column to adsorb organic impurities.

[0027] Described a kind of graphene modified adsor...

Embodiment 2

[0034] A kind of preparation method of acetaldehyde oxime, its operation step is:

[0035] According to the number of parts by mass, 50Kg hydroxylamine phosphate, 10.5Kg acetaldehyde and 320Kg water were added to the reactor, the temperature was controlled at 50°C, and the reaction mixture was obtained after 1 hour of reaction; The top of the tower is steamed, and the purified inorganic liquid at the bottom of the tower is returned to the former system for recycling to make hydroxylamine phosphate; while the top liquid of the stripping tower enters the rectification system for separation and purification, and finally obtains a 50% acetaldehyde oxime aqueous solution product; It is characterized in that the purification operation adopts a graphene-modified adsorbent packing adsorption column to adsorb organic impurities.

[0036] Described a kind of graphene modified adsorbent filler, its preparation method is as follows:

[0037] According to the mass parts, under the protect...

Embodiment 3

[0043] A kind of preparation method of acetaldehyde oxime, its operation step is:

[0044] According to the mass parts, 60Kg of hydroxylamine phosphate, 13.2Kg of acetaldehyde and 420Kg of water were added to the reactor, the temperature was controlled at 80°C, and the reaction mixture was obtained after 2 hours of reaction; The top of the tower is steamed, and the inorganic liquid purified at the bottom of the tower is returned to the front system for recycling to make hydroxylamine phosphate; while the top liquid of the stripping tower enters the rectification system for separation and purification, and finally obtains a 52% acetaldehyde oxime aqueous solution product; It is characterized in that the purification operation adopts a graphene-modified adsorbent packing adsorption column to adsorb organic impurities.

[0045] Described a kind of graphene modified adsorbent filler, its preparation method is as follows:

[0046] According to the mass parts, under nitrogen protec...

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Abstract

The invention relates to the field of chemical engineering, in particular to a preparation method of acetaldoxime. According to the preparation method of acetaldoxime, water is used as a solvent, hydroxylamine phosphate and acetaldehyde react to prepare acetaldoxime, the method is high in yield and simple in process, and hydroxylamine phosphate serving as a material is recycled; the method has theadvantages of the complex process, the short reaction flow, no byproduct, no use of toxic and harmful raw materials and less discharge of waste water and waste acid. A graphene modified adsorbent filler is adopted to refine a product solution, and the adsorbent resin has a very good adsorption effect on organic matter residues in wastewater, can be repeatedly recycled, and is greener, safer and more energy-saving compared with a traditional method used in the prior art.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of acetaldehyde oxime. Background technique [0002] Aldoxime is a reducing agent with low toxicity, a new type of oxygen scavenger with less pollution, low price and excellent oxygen scavenging effect. It is also an important organic synthesis and analysis reagent. In the 1990s, acetaldehyde oxime replaced the highly toxic hydrazine as a boiler water oxygen scavenger, and its oxygen scavenging effect was much higher than that of hydrazine, so it was widely used. [0003] 201811502082.4 involves a preparation method of acetaldehyde oxime. The preparation method of acetaldehyde oxime of the present invention comprises the following steps: 1) stirring and dissolving hydroxylamine and distilled water, then adding acetaldehyde and catalyst acetic acid dropwise under the condition of an ice-water bath; , to obtain acetaldehyde oxime solution; 2) the acetaldehyde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/08C07C249/14C07C251/38B01J20/20B01J20/30B01J20/34
CPCC07C249/08C07C249/14B01J20/20B01J20/3416B01J20/3475C07C251/38
Inventor 段仲刚周强江煜张则瑜王雄徐碧涛
Owner ZHEJIANG JINHUA NEW MATERIALS
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