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Method for recycling tetrafluoropropionamide from N,N-diethyl-2,3,3,3-tetrafluoropropylamine fluorination waste liquid

A technology of tetrafluoropropionamide and Ishikawa reagent, applied in the separation/purification of carboxylic acid amides, organic chemistry and other directions, can solve the problems such as reports of tetrafluoropropionamide documents and patents that have not been found, achieve high use value and reduce content , the effect of simple operation process

Active Publication Date: 2015-04-01
JIANGSU HANSYN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Although tetrafluoropropionamide is a by-product of the fluorination reaction, it also has unique uses in the electronics and pharmaceutical industries due to some special physical and chemical properties. caused great technical disadvantages
Up to now, by searching espacenet and Scifinder, no literature and patent reports on the purification of tetrafluoropropionamide have been found

Method used

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  • Method for recycling tetrafluoropropionamide from N,N-diethyl-2,3,3,3-tetrafluoropropylamine fluorination waste liquid
  • Method for recycling tetrafluoropropionamide from N,N-diethyl-2,3,3,3-tetrafluoropropylamine fluorination waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 500g of Ishikawa reagent fluorination waste liquid and 100g of water to a 2000ml four-necked reaction flask, which is equipped with a mechanical stirrer, a thermometer and an oil-water liquid container. Start the vacuum distillation, heat the material in the reaction flask to 60~70 through the oil bath o C. Control the vacuum degree to -0.08~-0.09MPa. The azeotrope of tetrafluoropropionamide and water is slowly distilled into the oil-water separator. The specific gravity of water is lighter than that of tetrafluoropropionamide. It will overflow from the oil-water separator. The mouth reaction flask continues to form an azeotrope with tetrafluoropropionamide, and the tetrafluoropropionamide is continuously distilled and recovered. The colorless and transparent liquid in the lower layer of the oil-water separator was collected to obtain 280 g of tetrafluoropropionamide with a recovery rate of 86%. GC chromatographic conditions: Agilent Gas Chromatography Model 7820; Co...

Embodiment 2

[0028] Add 200g of Ishikawa reagent fluorination waste liquid to a 500ml four-necked reaction flask, and add 100g of water to the dropping funnel. The four-neck reaction flask is equipped with a mechanical stirrer, a thermometer, an oil-water liquid container and a dropping funnel. Start the vacuum distillation, heat the material in the reaction flask to 70~80 through the oil bath o C. Control the vacuum degree to -0.08~-0.09MPa, and start to slowly add water from the dropping funnel. The azeotrope of tetrafluoropropionamide and water is slowly distilled into the oil-water separator at the same time. The specific gravity of water is four. The fluoropropanamide is light and will overflow from the oil-water separator to the four-necked reaction flask, continue to form an azeotrope with tetrafluoropropionamide, and continuously distill and recover the tetrafluoropropionamide. The colorless and transparent liquid in the lower layer of the oil-water separator was collected to obtain...

Embodiment 3

[0032] Add 100g of water to a 500ml four-necked reaction flask, and add 100g of Ishikawa reagent fluorination waste to the dropping funnel. The four-neck reaction flask is equipped with a mechanical stirrer, a thermometer, an oil-water liquid container and a dropping funnel. Start the vacuum distillation, heat the water in the reaction flask to 50~60 through the oil bath o C. Control the vacuum degree to -0.08~-0.09MPa, start to slowly drip the waste liquid of Ishikawa reagent fluorination from the dropping funnel, and the azeotrope of tetrafluoropropionamide and water is slowly distilled into the oil-water separator at the same time The specific gravity of water is lighter than that of tetrafluoropropionamide. It will overflow from the oil-water separator back to the four-necked reaction flask and continue to form an azeotrope with tetrafluoropropionamide. The tetrafluoropropionamide is continuously distilled and recovered. The colorless and transparent liquid in the lower lay...

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Abstract

The invention discloses a method for recycling tetrafluoropropionamide from an N,N-diethyl-2,3,3,3-tetrafluoropropylamine fluorination waste liquid. The method comprises the following steps: adding water into the N,N-diethyl-2,3,3,3-tetrafluoropropylamine fluorination waste liquid, then carrying out reduced pressure azeotropic distillation to recycle tetrafluoropropionamide, wherein the mass ratio of water to the N,N-diethyl-2,3,3,3-tetrafluoropropylamine fluorination waste liquid is (1-5) to 5; the preferable mass ratio is 1 to 2; the distillation temperature is 60-120 DEG C, preferably 70-80 DEG C; and the vacuum degree is controlled to be between -0.05MPa and -0.10MPa, preferably between -0.08 and -0.09MPa. The N,N-diethyl-2,3,3,3-tetrafluoropropylamine fluorination waste liquid is generated after carrying out fluoridation reaction on N,N-diethyl-2,3,3,3-tetrafluoropropylamine and a hydroxy compound. The N,N-diethyl-2,3,3,3-tetrafluoropropylamine used by the method is wide in source, is economic and is low in cost; the operation process is simple and liable to implement; the industrial amplification recycling is liable to implement; and the processed tetrafluoropropylamine is high in purity and has a high application value.

Description

technical field [0001] The invention relates to a method for recovering tetrafluoropropionamide from waste fluorination liquid of Ishikawa reagent, belonging to the field of industrial waste liquid treatment. Background technique [0002] Tetrafluoropropionamide is the well-known and most important by-product produced by Ishikawa reagent in the process of fluorination with hydroxyl compounds, and it is an important part of the fluorination waste liquid of Ishikawa reagent in pharmaceutical and chemical industry. [0003] Chinese name: N,N-diethyl-2,3,3,3-tetrafluoropropionamide, [0004] CAS #: 392-63-2, [0005] Chemical Structure: [0006] [0007] Ishikawa reagent is a fluorinating reagent commonly used in the fluorinating industry prepared from hexafluoropropylene and diethylamine. The mechanism of the by-product tetrafluoropropionamide in the fluorination process is as follows: [0008] [0009] Although tetrafluoropropionamide is a by-product of the fluorinati...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C233/05
Inventor 王喆丁尊良蒋成华
Owner JIANGSU HANSYN PHARMA
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