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Method for synthesizing N-acetylmorpholine

A technology for acetylmorpholine and morpholine, applied in the field of synthesizing N-acetylmorpholine, can solve the problems of large equipment investment, long reaction time, large energy consumption and the like, and achieves the advantages of small equipment investment, high production efficiency and low energy consumption. Effect

Inactive Publication Date: 2015-05-13
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for synthesizing N-acetylmorpholine, which solves the problem of high temperature, high energy consumption, large equipment investment and intermittent The problem of long reaction time and low yield

Method used

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  • Method for synthesizing N-acetylmorpholine
  • Method for synthesizing N-acetylmorpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) The rectification tower includes a tower kettle and a tower column. The tower kettle is a 500ml three-necked bottle, heated by an electric heating mantle, and the tower column is divided into three sections. The section and rectification section are Φ20mm glass tubes, the outer wall is coated with thermal insulation conductive film, the height of rectification section is 300mm, and stainless steel triangular packing is installed inside, the height of reaction section and dehydration section are 200mm and 400mm respectively, and Φ2*2mm ceramic ring is installed inside.

[0030] The upper end of the tower kettle is connected to the dehydration section, the dehydration section is connected to the reaction section, and the reaction section is connected to the rectification section. The upper and lower parts of the reaction section are respectively equipped with a feed port, which are respectively the upper feed port of the reaction section and the lower feed port of the re...

Embodiment 2

[0035] 1) The rectification tower includes a tower kettle and a tower column. The tower kettle is a 500ml three-necked bottle, heated by an electric heating mantle, and the tower column is divided into three sections. The section and rectification section are Φ20mm glass tubes, the outer wall is coated with thermal insulation conductive film, the height of rectification section is 300mm, and stainless steel triangular packing is installed inside, the height of reaction section and dehydration section are 200mm and 400mm respectively, and Φ2*2mm ceramic ring is installed inside.

[0036] The upper end of the tower kettle is connected to the dehydration section, the dehydration section is connected to the reaction section, and the reaction section is connected to the rectification section. The upper and lower parts of the reaction section are respectively equipped with a feed port, which are respectively the upper feed port of the reaction section and the lower feed port of the re...

Embodiment 3

[0041] 1) The rectification tower includes a tower kettle and a tower column. The tower kettle is a 500ml three-necked bottle, heated by an electric heating mantle, and the tower column is divided into three sections. The section and rectification section are Φ20mm glass tubes, the outer wall is coated with thermal insulation conductive film, the height of rectification section is 300mm, and stainless steel triangular packing is installed inside, the height of reaction section and dehydration section are 200mm and 400mm respectively, and Φ2*2mm ceramic ring is installed inside.

[0042] The upper end of the tower kettle is connected to the dehydration section, the dehydration section is connected to the reaction section, and the reaction section is connected to the rectification section. The upper and lower parts of the reaction section are respectively equipped with a feed port, which are respectively the upper feed port of the reaction section and the lower feed port of the re...

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Abstract

The invention relates to a method for synthesizing N-acetylmorpholine. The method comprises the following steps of adding N-acetylmorpholine, an acetic acid entrainer, a dehydrating agent and water into a tower bottom, heating until a residue is boiled, raising vapor, condensing, layering condensate into an oil phase and an aqueous phase, accumulating the aqueous phase in a layering device, refluxing the oil phase from an upper material inlet of a rectifying section, when the tower top temperature reaches 84.6 DEG C, adding morpholine from the upper material inlet of a reaction section, adding acetic acid from the lower material inlet of the reaction section, adding the acetic acid entrainer from the upper material inlet of a dehydrating section, reacting morpholine and acetic acid to produce morpholine salt, dehydrating morpholine salt to produce N-acetyl morpholine and water, azeotroping water and the dehydrating agent, passing through the dehydration section, the reaction section and rectifying section to enter the condenser for condensing, layering the condensate into the oil phase and an aqueous phase, extracting the aqueous phase, refluxing the oil phase and extracting N-acetylmorpholine from the tower bottom. The method for synthesizing N-acetylmorpholine is high in production efficiency, low in energy consumption, small in device investment, short in process and free of pollution and the large-scale continuous production can be achieved.

Description

technical field [0001] The invention relates to a method for synthesizing N-acetylmorpholine, which belongs to the field of chemistry. Background technique [0002] N-acetylmorpholine is an oxynitrogen heterocyclic compound, which is mainly used in the synthesis of medical and agricultural fungicides, aromatic hydrocarbon extractants and gas desulfurizers. The preparation method of N-acetylmorpholine is to take morpholine as raw material, and acetylating agent such as ketene (CN102295623), acetyl chloride (GB2223492), isopropenyl acetate (US2472633), acetic anhydride (CN200410069308, CN01128158) and acetic acid ( US 3558619), methyl acetate CA103641797) and other reactions, acetic acid has the best safety and the lowest price relative to other acylating agents. Therefore, the method for synthesizing N-acetylmorpholine from acetic acid and morpholine has attracted much attention. [0003] Acetic acid reacts with morpholine to synthesize N-acetylmorpholine. The first step gen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/185
CPCC07D295/185
Inventor 张晓杰苏宏李小刚王凤霞
Owner YANTAI UNIV
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