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Preparation process of 2,3,3,3-tetrafluoropropionic acid

A technology for the preparation of tetrafluoropropionic acid, which is applied in the fields of amide preparation, separation/purification of carboxylic acid compounds, metal/metal oxide/metal hydroxide catalysts, etc., and can solve the problem of difficult degradation of by-products and environmental pollution, etc. problems, to achieve the effect of facilitating product separation, reducing the generation of alkaline wastewater, and shortening the production cycle

Inactive Publication Date: 2018-08-03
佛山市飞程信息技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

N,N‐diethyl‐2,3,3,3‐tetrafluoropropionamide is the fluorinated product of N,N‐diethyl‐1,1,2,3,3,3‐hexafluoropropylamine By-product, the by-product is not easy to degrade, if it is discharged directly, it will seriously pollute the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Preparation of super strong solid base:

[0026] Add 14.8g of magnesium nitrate and 10.65g of aluminum nitrate to 30mL of water and 100mL of ethanol to make a solution, add 1mol / L Be(OH)2 to the solution, the pH value is 11, reflux for 36 hours, centrifuge, the precipitate is washed with water, and dried Overnight, under a nitrogen atmosphere, put the precipitate into a muffle furnace for high-temperature roasting at 800° C. for 3 hours to obtain a solid superbase catalyst A with a Be content of 1.32%.

[0027] 2) Put 6g of solid super base A, 200ml of water, 350ml of methanol and 60.3g of N,N-diethyl-2,3,3,3-tetrafluoropropionamide into a three-necked flask, stir and heat up to reflux at 100°C, After reacting for 20 hours, the catalyst was removed by filtration, the methanol was evaporated under normal pressure, and the reaction solution was lowered to about 1°C. A large amount of crystals were precipitated and separated by centrifugation to obtain 2,3,3,3‐tetrafluo...

Embodiment 2

[0029] 1) Preparation of super strong solid base:

[0030] Add 14.8g of magnesium nitrate and 8.52g of aluminum nitrate to 30mL of water and 100mL of ethanol to make a solution, add 1mol / L Be(OH)2 to the solution, the pH value is 11, reflux for 36 hours, centrifuge, and the precipitate is washed with water and dried Overnight, under a nitrogen atmosphere, put the precipitate into a muffle furnace for high-temperature roasting at 800° C. for 3 hours to obtain a solid superbase catalyst B with a Be content of 2.11%.

[0031] 2) Put 16g of solid super base B, 200ml of water, 350ml of methanol and 60.3g of N,N-diethyl-2,3,3,3-tetrafluoropropionamide into a three-necked flask, stir and heat up to reflux at 100°C, After reacting for 20 hours, the catalyst was removed by filtration, the methanol was evaporated under normal pressure, and the reaction liquid was lowered to about 1°C. A large amount of crystals were precipitated and centrifuged to obtain the product of 2,3,3,3-tetrafluo...

Embodiment 3

[0033] 1) Preparation of super strong solid base:

[0034] Add 14.8g of magnesium nitrate and 10.65g of aluminum nitrate to 30mL of water and 100mL of ethanol to make a solution, add 1mol / L Be(OH)2 to the solution, the pH value is 10, reflux for 36 hours, centrifuge, the precipitate is washed with water, and dried Overnight, under a nitrogen atmosphere, put the precipitate into a muffle furnace for high-temperature roasting at 800° C. for 3 hours to obtain a solid superbase catalyst C with a Be content of 2.33%.

[0035] 2) Put 15g of solid superbase C, 200ml of water, 350ml of methanol and 60.3g of N,N-diethyl-2,3,3,3-tetrafluoropropionamide into a three-necked flask, stir and heat up to reflux at 100°C, After reacting for 20 hours, the catalyst was removed by filtration, the methanol was evaporated under normal pressure, and the reaction liquid was lowered to about 1°C. A large amount of crystals were precipitated and centrifuged to obtain the product of 2,3,3,3-tetrafluorop...

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PUM

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Abstract

The invention relates to a preparation process of 2,3,3,3-tetrafluoropropionic acid. According to the method, the 2,3,3,3-tetrafluoropropionic acid is prepared by taking waste liquor containing N,N-diethyl-2,3,3,3-tetrafluoropropylamide as a raw material and taking beryllium-doped magnesium aluminum oxide solid super base as a catalyst under a hydrolysis condition. The molar yield is 99 percent ormore.

Description

technical field [0001] The invention provides a preparation method of a compound, specifically relates to a preparation process of 2,3,3,3-tetrafluoropropionic acid, and belongs to the technical field of chemical product preparation. Background technique [0002] 2,3,3,3-tetrafluoropropanoic acid (2,3,3,3-tetrafluoropropanoic acid), CAS No. 359-49-9, molecular formula C3H2F4O2, molecular weight 146, melting point 28.2°C, boiling point 120°C, is a widely used An important fluorine-containing intermediate used in the fields of medicine and pesticides. [0003] Hemer, I et al. (Journal of Fluorine Chemistry, 34(2), 241‐50; 1986) with 1,1‐dibromo‐1,2,2,2‐tetrafluoropropane or 1‐bromo‐1‐chloro‐1,2 , 2,2‐tetrafluoropropane as raw material, first reacts with zinc powder to form zinc reagent, then reacts with CO2 to introduce carboxyl groups, and finally debrominates or chlorinates under the action of zinc powder to synthesize 2,3,3,3‐tetrafluoropropane acid. The starting materia...

Claims

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Application Information

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IPC IPC(8): C07C51/06C07C51/43C07C53/21B01J23/02
CPCB01J23/02C07C51/06C07C51/43C07C53/21
Inventor 王飞利
Owner 佛山市飞程信息技术有限公司
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