Method for preparing octafluorovaleric acid under catalytic oxidation action of oxydol

A technology of catalytic oxidation and octafluorovaleric acid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve the problems of high price, insufficient selectivity, three wastes, etc., and achieves reduction of production cost, The effect of eliminating pollution sources and low prices

Active Publication Date: 2015-02-18
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The oxidizing agent can be air and pure oxygen. Although air and pure oxygen are easy to obtain, economical, cheap and non-corrosive, they have weak oxidizing ability and often need to be carried out under high temperature and pressure, and sometimes need to use corresponding catalysts. Not good enough, there are economic problems in the actual operation of the complete recovery of the catalyst
Therefore, other chemical reagents are often used, such as chromate, permanganate and periodide and other halogenated reagents with strong oxidizing properties. These oxidants often require equivalent or excessive amounts and are expensive, resulting in a large amount of three wastes.

Method used

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  • Method for preparing octafluorovaleric acid under catalytic oxidation action of oxydol
  • Method for preparing octafluorovaleric acid under catalytic oxidation action of oxydol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 136g (1.2mol) of hydrogen peroxide, 3.96g (0.012mol) of sodium tungstate and 3.87g (0.012mol) of tetrabutylammonium bromide with a content of 30% and place them in a magnetic stirring, reflux condenser, constant pressure feeding In a 1L flask with a funnel, an oil bath (normal temperature) and a thermometer, stir in an oil bath at 35°C for about 30 minutes to fully dissolve sodium tungstate and tetrabutylammonium bromide.

[0032] After raising the temperature to 85-90°C, 116 g (0.5 mol) of octafluoropentanol, the raw material, was added dropwise, and the vigorous stirring (500 r / min) was continued for 8 hours until the reaction was completed. Then continue to heat up the reaction solution and boil it, and check it with starch potassium iodide test paper until no blue color appears. Add 2.37g of BaCO 3 Powder, stirred for 1h, cooled slightly and filtered to remove solid precipitate. The colorless filtrate was concentrated to remove water by distillation under re...

Embodiment 2

[0035] Take by weighing 30% hydrogen peroxide 136g (1.2mol), 3g (0.012mol) tungstic acid (H 2 WO 4 ) and 1.08g (0.012mol) of oxalic acid were placed in a 1L flask equipped with magnetic stirring, reflux condenser, constant pressure addition funnel, oil bath (normal temperature) and thermometer, stirred in an oil bath at 40°C for 20min, fully Dissolve tungstic acid and oxalic acid.

[0036] After raising the temperature to 85-90°C, 116 g (0.5 mol) of octafluoropentanol, the raw material, was added dropwise, and the vigorous stirring (500 r / min) was continued for 8 hours until the reaction was completed. Then continue to heat up the reaction solution and boil it, and check it with starch potassium iodide test paper until no blue color appears. Add 2.37g of BaCO 3 Powder, stirred for 1h, cooled slightly and filtered to remove solid precipitate. The colorless filtrate was concentrated by distillation under reduced pressure to remove water, and then extracted three times with d...

Embodiment 3

[0039] Weigh 136g (1.2mol) of hydrogen peroxide with a content of 30%, 3.96g (0.012mol) of sodium tungstate and 3.73g (0.011mol) of tetrabutylammonium bisulfate and place them in a magnetic stirring, reflux condenser, constant pressure feeding In a 1L flask with a funnel, an oil bath (normal temperature) and a thermometer, stir in an oil bath at 35°C for about 30 minutes to fully dissolve sodium tungstate and tetrabutylammonium bisulfate.

[0040] After raising the temperature to 85-90°C, 139.2 g (0.6 mol) of octafluoropentanol, the raw material, was added dropwise, and the vigorous stirring (500 r / min) was continued for 8 hours until the reaction was completed. Then continue to heat up the reaction solution and boil it, and check it with starch potassium iodide test paper until no blue color appears. Add 2.37g of BaCO 3 Powder, stirred for 1h, cooled slightly and filtered to remove solid precipitate. The colorless filtrate was concentrated to remove water by distillation un...

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Abstract

The invention belongs to the field of organic chemistry, and relates to a method for preparing octafluorovaleric acid under the catalytic oxidation action of oxydol. The method comprises the following steps: 1) mixing oxydol, a phase-transfer catalyst or complexing agent and sodium tungstate in a mole ratio of 100:(0.7-1.2):(0.7-1.2), and heating the mixture to 85-90 DEG C; 2) adding octafluoropentanol into the mixture obtained in the step 1); and 3) adding BaCO3 powder to precipitate the sodium tungstate in the reaction mixture, stirring for 0.5-1.5 hours, cooling to 40-60 DEG C, and filtering to remove the precipitate. The invention provides an environment-friendly economically-feasible method for preparing octafluorovaleric acid; and by using the oxydol as the oxidizer, the reaction product is single, and the only expected reaction byproduct is water, thereby basically eliminating the pollution source of the oxidation process.

Description

technical field [0001] The invention belongs to the field of acyclic organic compounds, and in particular relates to a method for preparing polyfluorinated organic compounds. Background technique [0002] 2,2,3,3,3,4,4,5,5-octafluoropentanoic acid (alias: 5H-perfluoropentanoic acid) is an important class of organic fluorine intermediates, the English name is 2,2,3 ,3,3,4,4,5,5-Octafluorovaleric acid; Molecular formula is C 5 h 2 f 8 o 2 ; CAS No. 376-72-7. The structural formula of octafluorovaleric acid is shown in formula (I). [0003] [0004] Through the investigation of relevant literature at home and abroad, the oxidation of alcohols to acids is mainly divided into three types: chemical reagent oxidation, catalytic oxidation and electrolytic oxidation. The oxidizing agent can be air and pure oxygen. Although air and pure oxygen are easy to obtain, economical, cheap and non-corrosive, they have weak oxidizing ability and often need to be carried out under high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/21C07C51/285
CPCC07C51/285C07C51/42C07C53/21
Inventor 罗源军吕太勇刘波张鸣张建新
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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