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A method for recovering tetrafluoropropionamide from Ishikawa reagent fluorination waste liquid

A technology of tetrafluoropropionamide and Ishikawa reagent, which is applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems that have not yet been found in the literature and patent reports of tetrafluoropropionamide, achieve high use value and reduce processing Cost, the effect of overcoming technical difficulties

Active Publication Date: 2016-08-17
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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  • A method for recovering tetrafluoropropionamide from Ishikawa reagent fluorination waste liquid
  • A method for recovering tetrafluoropropionamide from Ishikawa reagent 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 into a 2000ml four-necked reaction flask equipped with a mechanical stirrer, a thermometer and an oil-water dispenser. Start vacuum distillation, and the material in the reaction bottle is heated to 60 ~ 70 by an 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, and it will overflow from the oil-water separator to Open the reaction bottle, continue to form an azeotrope with tetrafluoropropionamide, and continuously distill and recover tetrafluoropropionamide. The colorless transparent liquid of the lower floor of the oil-water separator was collected to obtain 280 g of tetrafluoropropionamide, and the recovery rate was 86%. GC chromatographic conditions: Agilent Gas Chromatography 7820 type; Chromatographic colu...

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-necked reaction flask is equipped with a mechanical stirrer, a thermometer, an oil-water dispenser and a dropping funnel. Start vacuum distillation, and the material in the reaction flask is heated to 70 ~ 80 by an oil bath o C, control the vacuum degree to -0.08~-0.09MPa, start to slowly add water from the dropping funnel, and the formed azeotrope of tetrafluoropropionamide and water is slowly distilled into the oil-water separator at the same time, and the specific gravity of water is four Fluoropropionamide is light, and will overflow from the oil-water separator back to the four-necked reaction flask, continue to form an azeotrope with tetrafluoropropionamide, and continuously distill and recover tetrafluoropropionamide. The colorless transparent liquid of the lower layer of the oil-water separator was collected to obt...

Embodiment 3

[0032] Add 100g of water to a 500ml four-necked reaction flask, and add 100g of Ishikawa reagent fluorination waste liquid to the dropping funnel. The four-necked reaction flask is equipped with a mechanical stirrer, a thermometer, an oil-water dispenser and a dropping funnel. Start vacuum distillation, and heat the water in the reaction flask to 50~60 by an oil bath o C, control the vacuum degree to -0.08~-0.09MPa, start to slowly drop the fluorinated waste liquid of Ishikawa reagent from the dropping funnel, and the formed 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 tetrafluoropropionamide, it will overflow from the oil-water separator back to the four-necked reaction flask, continue to form an azeotrope with tetrafluoropropionamide, and continuously distill and recover tetrafluoropropionamide. The colorless transparent liquid of the lower layer of the oil-wa...

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Abstract

The invention discloses a method for recovering tetrafluoropropionamide from waste fluorination liquid of Ishikawa reagent. Water is added to the waste fluoride liquid of Ishikawa reagent, followed by azeotropic distillation under reduced pressure to recover tetrafluoropropionamide. The mass ratio of water and Ishikawa reagent fluorination waste liquid is (1~5):5, and the preferred mass ratio is 1:2. The distillation temperature is 60-120°C, preferably 70-80°C. The degree of vacuum is controlled at -0.05Mpa~-0.10Mpa, preferably -0.08~-0.09MPa. The Ishikawa reagent fluorination waste liquid is the waste liquid produced after the Ishikawa reagent and hydroxyl compound undergo fluorination reaction. The Ishikawa reagent fluorination waste liquid used in the method has a wide range of sources, is economical and cheap, and the operation process is simple and easy, and is easy to be scaled up and recycled in an industrialized manner. The treated tetrafluoropropionamide has high purity and high use value.

Description

technical field [0001] The invention relates to a method for recovering tetrafluoropropionamide from fluorination waste 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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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C233/05
Inventor 王喆丁尊良蒋成华
Owner JIANGSU HANSYN PHARMA
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